连续自动再生化学抑制-离子色谱法测定石膏及其制品中的氟和氯

钟坚海; 郑瑞娟; 陈金凤; 陈章捷; 张艳燕; 林亚妹; 刘明健

doi:10.15898/j.cnki.11-2131/td.2015.03.012

连续自动再生化学抑制-离子色谱法测定石膏及其制品中的氟和氯

1.
国家矿产品检测重点实验室, 福建龙岩 364000

2.
龙岩出入境检验检疫局, 福建龙岩 364000

3.
龙岩学院化学与材料学院, 福建龙岩 364012

详细信息

作者简介: 钟坚海, 工程师, 从事色谱与光谱分析及相关研究.E-mail: 13850606002@163.com

中图分类号: O657.71;O613.41;O613.42

收稿日期: 2014-02-08

修回日期: 2015-05-07

录用日期: 2015-05-17

刊出日期: 2015-03-25

Determination of Fluoride and Chloride in Gypsum and Its Products by Ion Chromatograpy with Continuous Self-regenerated Chemical Suppressor

1.
State Key Testing Laboratory of Mineral, Longyan 364000, China

2.
China Longyan Entry-Exit Inspection and Quarantine Bureau, Longyan 364000, China

3.
College of Chemistry and Materials Science, Longyan University, Longyan 364012, China

Received Date: 08 February 2014

Revised Date: 07 May 2015

Accepted Date: 17 May 2015

Publish Date: 25 March 2015

摘要

摘要:
测定石膏及其制品中的氟化物和氯化物, 传统分析方法过程复杂, 分析速度慢, 准确度及灵敏度低。本文采用超声提取技术提取样品中的氟和氯, 以Na₂CO₃-NaHCO₃作为淋洗液, 色谱柱分离后通过抑制器降低背景电导, 用电导检测器进行检测。通过优化样品前处理和离子色谱分离条件, 在测定范围内氟和氯的含量与峰面积呈良好的线性关系(相关系数>0.9998), 方法检测限为0.15 ng/mL(氟)和0.28 ng/mL(氯), 加标回收率为95.0%~99.7%, 精密度(RSD)均小于5%(n=8)。本方法采用超声提取技术, 无需净化处理即可直接分析, 半小时内完成前处理, 且避免了目标分析物的损失。与离子选择电极法相比, 检测限由μg/mL提升至ng/mL级别。
- 石膏及其制品 /
- 氟化物 /
- 氯化物 /
- 超声提取 /
- 离子色谱法
Abstract:
Traditional determination of fluoride and chloride in gypsum and its products has the disadvantages of complicated pretreatment, long detection time, poor accuracy and low sensitivity. To remedy this, an ion chromatography method which can simultaneously determine the fluoride and chloride in gypsum and its products has been successfully developed. The sample was extracted firstly by ultrasonic processing and eluted by Na₂CO₃-NaHCO₃. The solution was then separated by anion column and suppressed by self-electric chemistry suppressor. Finally, the solution was detected using a conductivity detector. By optimizing the pretreatment and separate conditions, the concentrations of the fluoride and chloride have good linear relationships with the peak area in the measured range with correlation coefficients of 0.9999 and 0.9998 for F^- and Cl^-, respectively. The proposed method yielded the detection limits of 0.15 ng/mL and 0.28 ng/mL for F^- and Cl^-, respectively, the recovery of 95.0%-99.7% and the RSD of less than 5% (n=8). The proposed method utilizes ultrasonic extraction and avoids purification. The pretreatment can be completed in less than 0.5 h and the loss of target analyte can be avoided. Compared with the ion selective electrode method, the detection limit of this method improves from μg/mL to ng/mL.
- gypsum and its products /
- fluoride /
- chloride /
- ultrasonic extraction /
- Ion Chromatography

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图 1 样品浸出液稀释前后离子色谱图

Figure 1.

下载: 全尺寸图片幻灯片

表 1 淋洗液流速对目标离子分离结果的影响

Table 1. Effect of the flow velocity of eluting solution on anions separation

淋洗液流速 (mL/min)	保留时间 (min)		峰面积 (μS·min·cm^-1)		分离度
淋洗液流速 (mL/min)	F^-	Cl^-	F^-	Cl^-	分离度
0.3	7.91	11.96	0.61423	0.39410	1.75
0.5	4.76	7.21	0.36618	0.23519	2.25
0.7	3.42	5.17	0.26329	0.16848	1.70
0.9	2.68	4.05	0.20517	0.13262	1.34
1.1	2.22	3.35	0.16822	0.10895	1.49

下载: 导出CSV

表 2 柱温对目标离子分离结果的影响

Table 2. Effect of column temperature on anions separation

淋洗液流速 (mL/min)	保留时间 (min)		峰面积 (μS·min·cm^-1)		分离度
淋洗液流速 (mL/min)	F^-	Cl^-	F^-	Cl^-	分离度
15	3.4	5.44	0.26310	0.17062	1.85
20	3.4	5.34	0.26232	0.16873	1.76
25	3.41	5.25	0.26345	0.16911	1.67
30	3.41	5.18	0.26269	0.16849	1.60
35	3.43	5.11	0.26293	0.16762	1.52
40	3.44	5.06	0.26316	0.16941	1.47
45	3.45	5.02	0.26182	0.16828	1.42

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表 3 离子色谱法与离子选择电极法测定结果对比

Table 3. A comparison of analytical results by ion chromatography and ion selective electrode method

样品编号	目标离子	含量(mg/kg)
样品编号	目标离子	离子色谱法 (本法)	离子选择电极法
样品1	F^-	24.92	25.06
样品1	Cl^-	36.54	36.86
样品2	F^-	27.71	28.12
样品2	Cl^-	80.91	79.98
样品3	F^-	341.72	342.77
样品3	Cl^-	515.77	517.65

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连续自动再生化学抑制-离子色谱法测定石膏及其制品中的氟和氯

1. 国家矿产品检测重点实验室, 福建 龙岩 364000 2. 龙岩出入境检验检疫局, 福建 龙岩 364000 3. 龙岩学院化学与材料学院, 福建 龙岩 364012

作者简介: 钟坚海, 工程师, 从事色谱与光谱分析及相关研究.E-mail: 13850606002@163.com

Determination of Fluoride and Chloride in Gypsum and Its Products by Ion Chromatograpy with Continuous Self-regenerated Chemical Suppressor

1. State Key Testing Laboratory of Mineral, Longyan 364000, China 2. China Longyan Entry-Exit Inspection and Quarantine Bureau, Longyan 364000, China 3. College of Chemistry and Materials Science, Longyan University, Longyan 364012, China

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目录

1.
国家矿产品检测重点实验室, 福建龙岩 364000

2.
龙岩出入境检验检疫局, 福建龙岩 364000

3.
龙岩学院化学与材料学院, 福建龙岩 364012

1.
State Key Testing Laboratory of Mineral, Longyan 364000, China

2.
China Longyan Entry-Exit Inspection and Quarantine Bureau, Longyan 364000, China

3.
College of Chemistry and Materials Science, Longyan University, Longyan 364012, China