CN102221594A - Method for determining hexylene diamine content in water by using gas chromatography method - Google Patents
Method for determining hexylene diamine content in water by using gas chromatography method Download PDFInfo
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- CN102221594A CN102221594A CN2011100886362A CN201110088636A CN102221594A CN 102221594 A CN102221594 A CN 102221594A CN 2011100886362 A CN2011100886362 A CN 2011100886362A CN 201110088636 A CN201110088636 A CN 201110088636A CN 102221594 A CN102221594 A CN 102221594A
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- hexane diamine
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Abstract
The invention relates to a method for determining hexylenediamine content in water by using a gas chromatography (GC) method. The method comprises the steps: adding sodium hydroxide to a water sample for alkalizing, extracting by using toluene, drying an organic layer by blowing, restricting the volume by using toluene, and carrying out derivation by using heptafluorobutyric anhydride; weighing a standard hexylene diamine sample, dissolving the sample by using toluene, weighing the dissolved sample, wherein the sample is then regarded as a mass concentration stock solution; dissolving the stock solution by using toluene, such that a standard working solution with concentration gradient is obtained; carrying out derivation by using heptafluorobutyric anhydride; testing the treated sample solution by using a gas chromatograph, and results can be obtained through calculating. With the method provided by the present invention, the hexylene diamine content in water can be detected quickly and effectively, with a linearity range of 5[mu]g/L to 200[mu]g/L, and a relative average deviation smaller than 5.0%. Therefore, the present invention provides a reliable and effective method for determining the hexylene diamine content in water. The method satisfies the requirements of researching, producing and environment monitoring.
Description
Technical field
The present invention relates to hexane diamine Determination on content method in a kind of water, particularly relate to a kind of vapor-phase chromatography hexane diamine Determination on content method in the water.
Background technology
Hexane diamine (1,6-Diaminohexane; Hexamethylene diamine) is mainly used in the synthetic important industrial products nylon 66 of hexane diacid.Can be used to produce polyurethane resin, epoxy resin, cementing agent and crosslinking chemical or the like in addition.This material belongs to strong toxicant, can cause the change of nervous system, antiotasis and hematopoiesis function, is 0.0027mg/m to the photosensitive threshold of eye
3, olfactory threshold is 0.0033mg/m
3Workplace maximum permissible concentration 1mg/m
3In production, use and the offal treatment process of hexane diamine and products thereof, discharging contains waste water, waste gas and the waste residue of hexane diamine, causes that serious environmental is polluted and harm.At present domestic do not have in addition a kind of specially at hexane diamine content detecting method in the water.Therefore set up a kind of quick, accurate, convenient and economic detection method, help monitoring hexane diamine production and use near the water quality enterprise, thus guarantee employee and popular Environmental security.
Summary of the invention
Technical matters to be solved by this invention is, overcome the not high higher defective of detection limit that causes of hexane diamine response in other instruments, provide hexane diamine Determination on content method in a kind of use gas Chromatographic Determination water by fishing for the suitable method of sampling, best derivative reagent and optimum chromatogram condition.
For achieving the above object, the present invention takes following design proposal:
A kind of vapor-phase chromatography of the present invention comprises the steps: hexane diamine Determination on content method in the water
Measure the 100ml water sample in separating funnel, add 50g NaOH in water sample, stirring is dissolved it fully, places room temperature.Add 50ml toluene, concuss 2min leaves standstill, treat layering after, get organic phase in the heart bottle, extract once with 25ml toluene again, merge organic phase.Be spin-dried under 65 ℃, add 2ml toluene constant volume, add 100 μ l heptafluorobutyric anhydrides again, mixing, the 70min that derives under 55 ℃, be cooled to room temperature after, cross the 0.45um filter membrane, treat gas chromatographic analysis.
Taking by weighing the hexane diamine standard items, as the mass concentration storing solution, is the standard use liquid with concentration gradient with dilution with toluene further with toluene dissolving and the back of weighing then;
Utilize gas chromatograph that titer and sample treatment solution are detected;
Result of calculation, the computing formula of hexane diamine content is in the sample:
In the formula:
The content of X---hexane diamine, unit are every liter of microgram (μ g/L);
C---hexane diamine concentration in the sample, unit is μ g/mL;
C
0---hexane diamine concentration in the blank, unit is μ g/mL;
V
1---constant volume, mL;
V
2---volume of water sample, mL.
Preferably, described alkalizing agent is a NaOH, and addition is 50g/100ml.
Preferably, organic extractant is selected toluene for use.
Preferably, described sample to be tested adopts mass concentration to operate and calculate in whole preparation process.
Preferably, use heptafluorobutyric anhydride to be derivative reagent.
The described gas chromatograph that utilizes to the condition that sample treatment solution detects is:
Chromatographic column: DB-1,30m * 0.25mm (internal diameter), 0.25 μ m (thickness)
Injector temperature: 250 ℃;
Split ratio: 5: 1
Sampling volume: 1.0 μ L;
Column temperature: 60 ℃ (keeping 0min), be warming up to 200 ℃ (keeping 2min) with 10 ℃/min,
Be warming up to 270 ℃ (keeping 5min) with 30 ℃/min
Flow velocity: 1.00mL/min;
Detecting device: electron capture detector (ECD);
Detector temperature: 300 ℃.
And qualitative according to retention time, the external standard peak area method is quantitative.
Advantage of the present invention is: adopt method of the present invention to detect the content of hexane diamine in the water, effectively, RSD is less than 5% fast, and the range of linearity is 5ug/L-200ug/L, detects to be limited to 5ug/L.This shows that method of the present invention be to detect the content of hexane diamine in the water body, a kind of method of implementing be convenient to reliably be provided, can satisfy research and produce in needs.
Embodiment
Embodiment 1, and the precision of hexane diamine content and the recovery detect in the water:
Measure the 100ml water sample in separating funnel, add 50g NaOH in water sample, stirring is dissolved it fully, places room temperature.Add 50ml toluene, concuss 2min leaves standstill, treat layering after, get organic phase in the heart bottle, extract once with 25ml toluene again, merge organic phase.Be spin-dried under 65 ℃, add 2ml toluene constant volume, add 100 μ l heptafluorobutyric anhydrides again, mixing, the 70min that derives under 55 ℃, be cooled to room temperature after, cross the 0.45um filter membrane, treat gas chromatographic analysis.
Take by weighing hexane diamine standard items (purity 99.5% U.S. Aldrick) 10.00mg, with toluene dissolving and be settled to 10.00mL, obtain the standard reserving solution that concentration is 1000mg/mL, further use liquid with 50 times of dilution with toluene as standard then, dilution is 1.0,5.0,10.0 again, the standard of 50.0mg/mL uses liquid.
Detecting instrument is that existing Agilent 7890 gas chromatographs are equipped with electron capture detector:
Testing conditions is:
Chromatographic column: DB-1,30m * 0.25mm (internal diameter), 0.25 μ m (thickness)
Injector temperature: 250 ℃;
Split ratio: 5: 1
Sampling volume: 1.0 μ L;
Column temperature: 60 ℃ (keeping 0min), be warming up to 200 ℃ (keeping 2min) with 10 ℃/min,
Be warming up to 270 ℃ (keeping 5min) with 30 ℃/min;
Flow velocity: 1.00mL/min;
Detecting device: electron capture detector (ECD);
Detector temperature: 300 ℃.
Qualitative according to retention time, the external standard peak area method is quantitative.
Result of calculation, the computing formula of hexane diamine content is in the sample:
In the formula:
The content of X---hexane diamine, unit are every liter of microgram (μ g/L);
C---hexane diamine concentration in the sample, unit is μ g/mL;
C
0---hexane diamine concentration in the blank, unit is μ g/mL;
V
1---constant volume, mL;
V
2---volume of water sample, mL.
Through calculating, the result is:
In the sample content of hexane diamine by formula (1) calculate, the result is as follows:
Obviously, those of ordinary skill in the art can use gas chromatograph that the content of hexane diamine in the water is measured according to step of the present invention.
The foregoing description is only for the usefulness that the present invention is described; and be not to be limitation of the present invention; the those of ordinary skill in relevant technologies field; without departing from the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also should belong to category of the present invention, and scope of patent protection of the present invention should be limited by each claim.
Claims (6)
1. a vapor-phase chromatography is to hexane diamine Determination on content method in the water, and it is characterized in that: described assay method comprises the steps:
Measure the 100ml water sample in separating funnel, add 50g NaOH in water sample, stirring is dissolved it fully, places room temperature.Add 50ml toluene, concuss 2min leaves standstill, treat layering after, get organic phase in the heart bottle, extract once with 25ml toluene again, merge organic phase.Be spin-dried under 65 ℃, add 2ml toluene constant volume, add 100 μ l heptafluorobutyric anhydrides again, mixing, the 70min that derives under 55 ℃, be cooled to room temperature after, cross the 0.45um filter membrane, treat gas chromatographic analysis.
Taking by weighing the hexane diamine standard items, as the mass concentration storing solution, is the standard use liquid with concentration gradient with dilution with toluene further with toluene dissolving and the back of weighing then;
Utilize gas chromatograph to use liquid and sample treatment solution to detect to standard;
Result of calculation, the computing formula of hexane diamine content is in the sample:
In the formula:
The content of X---hexane diamine, unit are every liter of microgram (μ g/L);
C---hexane diamine concentration in the sample, unit is μ g/mL;
C
0---hexane diamine concentration in the blank, unit is μ g/mL;
V
1---constant volume, mL;
V
2---water sample sample volume, mL.
2. a kind of vapor-phase chromatography according to claim 1 is to hexane diamine Determination on content method in the water, it is characterized in that: described adding 50g NaOH carries out alkalizing solution, can guarantee the basicity of solution, guaranteed that simultaneously hexane diamine exists with molecular state, easier of organic solvent extraction, guaranteed the recovery of object.
3. a kind of vapor-phase chromatography according to claim 1 is to hexane diamine Determination on content method in the water, it is characterized in that: use toluene as organic extraction agent, guarantee that hexane diamine can well be by this kind organic solvent extraction, the while can the masked segment interfering material.
According to the described a kind of vapor-phase chromatography of claim 1 to hexane diamine Determination on content method in the water, it is characterized in that: used heptafluorobutyric anhydride as derivative reagent, the derivant that produces has good response being equipped with on the gas chromatography of electron capture detector, detection limit is low.
5. a kind of vapor-phase chromatography according to claim 1 is characterized in that hexane diamine Determination on content method in the water: the described gas chromatograph that utilizes to the condition that sample treatment solution and standard solution detect is:
Chromatographic column: DB-1,30m * 0.25mm (internal diameter), 0.25 μ m (thickness)
Injector temperature: 250 ℃;
Split ratio: 5: 1
Sampling volume: 1.0 μ L;
Column temperature: 60 ℃ (keeping 0min), be warming up to 200 ℃ (keeping 2min) with 10 ℃/min,
Be warming up to 270 ℃ (keeping 5min) with 30 ℃/min
Flow velocity: 1.00mL/min;
Detecting device: electron capture detector (ECD);
Detector temperature: 300 ℃.
Has good separating effect under this condition.
6. a kind of vapor-phase chromatography according to claim 1 is characterized in that hexane diamine Determination on content method in the water: utilize comparatively general, suitable gas chromatograph that the content of hexane diamine in the water is detected.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100886362A CN102221594A (en) | 2011-04-11 | 2011-04-11 | Method for determining hexylene diamine content in water by using gas chromatography method |
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| CN2011100886362A CN102221594A (en) | 2011-04-11 | 2011-04-11 | Method for determining hexylene diamine content in water by using gas chromatography method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370610A (en) * | 2016-08-31 | 2017-02-01 | 四川北方红光特种化工有限公司 | Method of detecting content of trace phenol in nitro-o-xylene |
| CN106596796A (en) * | 2017-01-09 | 2017-04-26 | 国家烟草质量监督检验中心 | Method for detecting 9 aromatic amines in mainstream smoke of cigarettes with GC-MS (gas chromatography-mass spectrometry) based on liquid-liquid micro-extraction |
| CN110749676A (en) * | 2019-10-30 | 2020-02-04 | 深圳天祥质量技术服务有限公司 | Detection method for migration amounts of ethylenediamine and hexamethylenediamine in food contact material and product |
| CN113176372A (en) * | 2021-05-20 | 2021-07-27 | 北京化工大学 | Gas chromatography method for detecting content of adipic acid in fermentation liquor |
| CN116973343A (en) * | 2023-07-04 | 2023-10-31 | 岭南师范学院 | Method for detecting hexamethylenediamine |
-
2011
- 2011-04-11 CN CN2011100886362A patent/CN102221594A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 刘尔嘉 等: "废水和大气中痕量己二胺的气相色谱分析", 《化工环保》 * |
| 王莹 等: "气相色谱分析己二胺残夜液", 《分析实验室》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106370610A (en) * | 2016-08-31 | 2017-02-01 | 四川北方红光特种化工有限公司 | Method of detecting content of trace phenol in nitro-o-xylene |
| CN106370610B (en) * | 2016-08-31 | 2019-05-14 | 四川北方红光特种化工有限公司 | The detection method of micro phenol content in a kind of nitro ortho-xylene |
| CN106596796A (en) * | 2017-01-09 | 2017-04-26 | 国家烟草质量监督检验中心 | Method for detecting 9 aromatic amines in mainstream smoke of cigarettes with GC-MS (gas chromatography-mass spectrometry) based on liquid-liquid micro-extraction |
| CN110749676A (en) * | 2019-10-30 | 2020-02-04 | 深圳天祥质量技术服务有限公司 | Detection method for migration amounts of ethylenediamine and hexamethylenediamine in food contact material and product |
| CN113176372A (en) * | 2021-05-20 | 2021-07-27 | 北京化工大学 | Gas chromatography method for detecting content of adipic acid in fermentation liquor |
| CN116973343A (en) * | 2023-07-04 | 2023-10-31 | 岭南师范学院 | Method for detecting hexamethylenediamine |
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Application publication date: 20111019 |