【摘要】：本論文提出了TPTZ-Fe~(2+)顯色體系-流動(dòng)注射分光光度法測定水汽中的痕量鐵含量。通過將流動(dòng)注射分析儀與紫外監(jiān)測器、高溫自動(dòng)加熱密閉消解模塊聯(lián)用,利用TPTZ與二價(jià)鐵顯色反應(yīng)的方法,實(shí)現(xiàn)了全封閉實(shí)時(shí)在線測定電廠水汽中的總鐵含量。實(shí)驗(yàn)研究了試劑條件優(yōu)選和水樣消解條件優(yōu)選以及p H值對系統(tǒng)測定的影響,完成了消解、化學(xué)反應(yīng)、檢測三大塊實(shí)驗(yàn)臺(tái)搭建并進(jìn)行了初步應(yīng)用,結(jié)果表明本方法所測定電廠水汽中的總鐵準(zhǔn)確度較高。1、試劑條件優(yōu)選。(1)總鐵濃度在0-80mg/L范圍內(nèi),抗壞血酸濃度為10mg/L,TPTZ濃度為40mg/L。高量程鐵在優(yōu)選時(shí)分成了兩個(gè)階段,總鐵濃度在0-1mg/L范圍內(nèi)時(shí),抗壞血酸濃度為20mg/L,TPTZ濃度為80mg/L;總鐵濃度在1-3.5mg/L的范圍內(nèi)時(shí),抗壞血酸濃度為40mg/L,TPTZ濃度為240mg/L。配制100mg/L硫酸鐵銨母液所用HCl濃度優(yōu)選。(2)測定試樣鐵離子濃度范圍在0-100ug/L,選擇用4mol/L或者5mol/L鹽酸,測定試樣鐵離子濃度大于100ug/L時(shí),選擇1mol/L的鹽酸。2、p H值對系統(tǒng)測定的影響。采用不同方法探索了待測試樣酸度對靈敏度的影響,實(shí)際檢測過程中應(yīng)使試樣p H值在最適宜的范圍內(nèi),當(dāng)檢測試樣的總鐵含量大于100ug/L時(shí)可以適當(dāng)拓寬p H值范圍,在2.3-3.5之間,當(dāng)含量為小于等于100ug/L時(shí)則盡量將檢測試樣p H值控制在2.3-3之間。3、水樣消解條件優(yōu)選。90℃水浴加熱條件下,加0.1m L消解液,消解10min即可消解完全。在此實(shí)驗(yàn)數(shù)據(jù)的基礎(chǔ)上確定了在線消解實(shí)驗(yàn)停留時(shí)間、加熱模塊溫度、泵管內(nèi)徑、泵速等條件,優(yōu)選出的停留時(shí)間10min,對應(yīng)的蠕動(dòng)泵擋位為1擋,泵速為5r/min,在此擋位下總流量為1m L/min,冷卻盤管可以將消解后的高溫液體冷卻到室溫。泵管徑為酸路管徑為0.38mm,水樣路管徑為2.58mm。4、將消解、化學(xué)反應(yīng)、檢測三大塊實(shí)驗(yàn)臺(tái)搭建完整,并利用該系統(tǒng)對張家口宣化熱電啟動(dòng)機(jī)組的爐水實(shí)際水樣進(jìn)行測定,與哈希標(biāo)準(zhǔn)測定方法作比較,相對誤差在2%左右,結(jié)果顯示本方法所測定電廠水汽中的總鐵準(zhǔn)確度較高。
[Abstract]:In this paper, a TPTZ-Fe~ (2) color system-flow injection spectrophotometry was proposed for the determination of trace iron in water vapor. By combining the flow injection analyzer with UV monitor and high temperature automatic heating closed digestion module, the total iron content in water vapor of power plant was determined on-line by using the method of color reaction of TPTZ with divalent iron. The effects of reagent condition optimization, water sample digestion condition optimization and pH value on the systematic determination were studied experimentally. the digestion, chemical reaction and detection three experimental platforms were built and applied. The results show that the accuracy of the determination of total iron in water vapor of power plant is high. 1. The reagent conditions are optimized. (1) in the range of 0-80mg/L, the concentration of ascorbic acid is 10 mg 路L and the concentration of TPTZ is 40 mg 路L ~ (- 1). The high range iron was divided into two stages. When the total iron concentration was in the range of 0-1mg/L, the concentration of ascorbic acid was 20 mg 路L and the concentration of TPTZ was 80 mg 路L, and the concentration of ascorbic acid was 20 mg 路L ~ (- 1) and the concentration of TPTZ was 80 mg 路L ~ (- 1). When the total iron concentration is within the range of 1-3.5mg/L, the concentration of ascorbic acid is 40 mg 路L and the concentration of TPTZ is 240 mg 路L ~ (- 1). The concentration of HCl used in the preparation of 100mg/L ammonium iron sulfate mother liquor was optimized. (2) the concentration range of iron ion in the sample was 0 渭 g 路L ~ (- 1), and the concentration of iron ion in the sample was higher than 100ug/L when the concentration of iron ion was 0 渭 g 路L ~ (- 1), 4mol/L or 5mol/L hydrochloric acid was selected. The effect of hydrochloric acid. 2, pH value of 1mol/L on the determination of the system was selected. The influence of acidity on the sensitivity of the sample to be tested was explored by different methods. The pH value of the sample should be made in the most suitable range in the actual detection process, and the range of pH value could be widened appropriately when the total iron content of the sample was greater than 100ug/L. In the range of 2.3 鈮，

本文編號(hào)：2481351