本文選題：非抑制型離子色譜 + 同時(shí)分離��； 參考：《北京化工大學(xué)》2008年碩士論文

【摘要】： 在爆炸現(xiàn)場,對(duì)爆炸殘留物進(jìn)行檢測,對(duì)鑒別無機(jī)爆炸物的種類是非常重要的。本文研究了用便攜式非抑制型離子色譜儀島津PIA-1000對(duì)爆炸物殘留中的無機(jī)陰、陽離子進(jìn)行了同時(shí)分離和檢測。在最優(yōu)的色譜條件下,16 min內(nèi)可對(duì)8種無機(jī)陰陽離子(Cl~-,NO_2~-,NO_3~-,ClO_3~-,SO_4~(2-),K~+,Na~+,NH_4~+)進(jìn)行同時(shí)分離和檢測,并將此方法應(yīng)用到實(shí)際爆炸物樣品的檢測中,可以滿足對(duì)現(xiàn)場爆炸物殘留的無機(jī)陰、陽離子的定性、定量分析。在本試驗(yàn)中主要考慮到了以下幾個(gè)因素: 1、選擇合適的淋洗液。所選擇的淋洗液必須同時(shí)具有疏水性功能基團(tuán)和親水性功能基團(tuán),與陰離子交換柱和陽離子交換柱的功能基團(tuán)相結(jié)合,對(duì)無機(jī)陰、陽離子進(jìn)行離子交換作用。本實(shí)驗(yàn)中選擇了鄰苯二甲酸作為淋洗液。 2、考慮淋洗液的pH值對(duì)整個(gè)分離過程的影響。淋洗液鄰苯二甲酸有兩個(gè)不同的pKa值,在不同的pH值下,它會(huì)表現(xiàn)出不同的離子形態(tài),擁有不同的離子交換強(qiáng)度,必須選擇了合適的pH值,使淋洗液有合適的離子強(qiáng)度。 3、考慮了鄰苯二甲酸的濃度對(duì)分離過程的影響。隨著濃度的增加,可交換的離子增加,離子交換能力變大,但隨著濃度的增加,背景電導(dǎo)也增加,降低了分析的靈敏度。因此必須找到一個(gè)合適的濃度,使淋洗液擁有足夠的離子交換能力和靈敏度。 4、研究了有機(jī)添加劑乙腈在淋洗液中的含量對(duì)分離過程的影響。淋洗液中乙腈含量增加,可以增加淋洗液的疏水性,乙腈還可以占據(jù)柱子固定相中的疏水空腔,減少目標(biāo)離子和柱子的非離子交換作用,從而改善目標(biāo)離子的峰形,分離度和保留時(shí)間。 5、研究了陰陽離子交換柱的連接順序?qū)φ麄�(gè)分離過程的影響。 最后,得到了同時(shí)對(duì)8種無機(jī)陰、陽離子分離的最佳條件是:鄰苯二甲酸濃度3.5 mM,pH=4.0,乙腈加入量2%,柱子連接順序?yàn)殛庪x子交換柱-陽離子交換柱。 在最優(yōu)的色譜條件下,可以在16 min內(nèi)對(duì)8種無機(jī)陰、陽離子進(jìn)行完全的分離,并把此方法應(yīng)用到實(shí)際爆炸物樣品的檢測中。。
[Abstract]:At the scene of the explosion, the detection of explosive residues is very important for the identification of inorganic explosives.In this paper, the simultaneous separation and determination of inorganic anions and cations in explosive residue by PIA-1000, a portable uninhibited ion chromatograph, were studied.Under the optimal chromatographic conditions, 8 kinds of inorganic anions, Cl-No _ 2H _ 2N _ 2H _ 2O _ 3H _ O _ 3H _ O _ 3H _ O _ 3H _ O _ 3O _ 3O _ 3O _ 3 / S _ 4T _ 4 can be separated and detected simultaneously within 16 min. The method has been applied to the detection of real explosives samples, and can satisfy the inorganic negative of explosive residue in the field, and can be applied to the detection of real explosive samples, and the method can be applied to the detection of practical explosives samples, and the method can be applied to the detection of explosives in the field.Qualitative and quantitative analysis of cations.The following factors have been taken into account in this experiment:1. Choose the appropriate eluent.The eluant must have hydrophobic and hydrophilic groups, which are combined with the functional groups of anion exchange column and cation exchange column to exchange inorganic anions and cations.In this experiment, phthalic acid was selected as eluent.2. The effect of pH value of eluate on the whole separation process was considered.Phthalic acid has two different pKa values. Under different pH values, phthalic acid has different ionic forms and different ion exchange intensities. It is necessary to select the appropriate pH value to make the eluent have appropriate ionic strength.3. The influence of phthalic acid concentration on the separation process was considered.With the increase of the concentration, the exchangeable ions increase and the ion exchange ability increases, but with the increase of the concentration, the background conductance also increases, which reduces the sensitivity of the analysis.Therefore, a suitable concentration must be found so that the eluent has sufficient ion exchange capacity and sensitivity.4. The effect of the content of acetonitrile on the separation process was studied.The increase of acetonitrile content in the eluate can increase the hydrophobicity of the eluate. Acetonitrile can also occupy the hydrophobic cavity in the stationary phase of the column and reduce the non-ion exchange between the target ion and the column, thus improving the peak shape of the target ion.Separation degree and retention time.5. The influence of the connection sequence of cationic ion exchange column on the whole separation process was studied.Finally, the optimum conditions for the separation of eight inorganic anions were obtained as follows: the concentration of phthalic acid was 3.5 mm ~ (-1) pH ~ (+) 4.0, the amount of acetonitrile was 2 ~ (th), and the column connection sequence was anion exchange column and cation exchange column.Under the optimum chromatographic conditions, eight inorganic anions and cations could be completely separated in 16 min, and the method was applied to the detection of real explosives.
【學(xué)位授予單位】：北京化工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2008
【分類號(hào)】：D918.91

【引證文獻(xiàn)】

相關(guān)碩士學(xué)位論文 前2條

1 方芳;二氟乙酰乙酸乙酯合成過程質(zhì)量監(jiān)控體系的建立[D];華東理工大學(xué);2011年

2 戴慧;含氟有機(jī)化合物的離子色譜研究[D];中南大學(xué);2011年

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本文編號(hào)：1762852