Research on Pre-Treatment Technology and Analysis Methods for Main Components in Soluble Potassium Salt
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摘要:
钾盐是中国最紧缺的矿产资源之一，为农业三大肥料中钾肥的主要原料，当前具有开发利用价值的主要是可溶性钾盐资源。而目前可溶性钾盐尚无国家标准物质和标准分析方法，本文对称样量、固液比、溶解温度、溶解时间、搅拌条件、超声时间和功率等条件进行实验研究，利用电热板和超声振荡两种溶解方式，建立了可溶性钾盐中主要成分钾、钠、钙、镁、氯和硫酸根离子的分析方法。采用电感耦合等离子体发射光谱仪测定样品中的Ca2+、Mg2+ 、K+和Na+的含量，离子色谱仪测定样品中Cl−和SO4 2−的含量，两种溶解方法分析可溶性钾盐样品中上述离子的实验结果基本吻合。电热板溶解方法精密度为0.52%～3.19%(RSD，n=11)，超声振荡溶解方法精密度为0.55%～3.07%(RSD，n=11)，两种方法检出限为0.01～0.05μg/g。利用主要成分百分含量加和、加标回收率、阴阳离子平衡验证方法准确性，两种溶解方法的主要成分加和在99.0％～101.0％之间，加标回收率 在95.3%～103.8%，阴阳离子平衡在−3%～3%之间，均满足DZ/T 0130.3—2006质量管理规范中的分析要求。两种可溶性钾盐的溶解方法均可在日常检测中应用，对于较大批的钾盐样品分析，电热板溶解法整体工作效率较高，更适用于实验室内批量样品分析；超声振荡器溶解方法与电热板溶解方法相比，更为简单快速，对于少量样品的分析，效率更高，且超声波振荡器方便野外携带，使用在钾盐的野外现场勘探工作中，可较大地提高工作效率，实时指导找矿行动顺利开展。
Abstract:Potassium salt is one of the scarcest mineral resources in China, and it is the main raw material for potassium fertilizer in the three major fertilizers of agriculture. Currently, soluble potassium salt resources are the main ones with development and utilization value. At present, there is no national standard material or standard analysis method for soluble potassium salts. In the experiments, soluble potassium salt samples were dissolved by electric heating plate and ultrasonic oscillation. According to the main components of soluble potassium salts, a method for the determination of K+, Na+, Ca2+ and Mg2+ by ICP-OES and a method for the determination of Cl− and SO4 2− by ion chromatography (IC) in soluble potassium salts were established. Through experimental conditions, the dissolution temperature of the electric heating plate was determined to be 160℃ and slightly boiled for 20min; the ultrasonic oscillation dissolution power was 60Hz and the time was 20min. The precision of the two methods was between 0.55%−3.19% (RSD, n=11), and the detection limit was between 0.01μg/g to 0.05μg/g. Both dissolution methods of soluble potassium salts can be widely used in daily detection. The electric heating plate dissolution method is more suitable for batch sample analysis in the laboratory. The ultrasonic oscillator dissolution method is simple and fast, and can be widely used in the field exploration of potassium salts, which can greatly improve the work efficiency and guide the smooth development of prospecting operations in real time.
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表 1 电热板溶解法和超声振荡溶解法不同称样量下主要成分的测定结果
Table 1. Measurement results of main components pretreated with electric heating plate dissolution method and ultrasonic oscillation dissolution method under different sample sizes
实验样品 称样量
(g)电热板溶解法中主要成分的测定值(%) 超声振荡溶解法中主要成分的测定值(%) K+ Na+ Ca2+ Mg2+ Cl− SO4 2− K+ Na+ Ca2+ Mg2+ Cl− SO4 2− 样品A 1.0000 10.95 27.11 0.014 0.015 45.29 4.65 10.93 26.97 0.014 0.013 45.91 4.69 2.0000 10.94 27.08 0.016 0.013 45.80 4.86 10.75 27.07 0.016 0.014 45.55 4.97 4.0000 11.11 26.97 0.015 0.013 46.03 4.48 10.69 27.39 0.014 0.013 45.27 4.55 样品B 1.0000 14.86 23.60 0.019 0.011 39.33 12.37 14.78 23.93 0.018 0.011 39.71 12.39 2.0000 14.90 23.58 0.018 0.011 39.80 12.74 14.90 23.81 0.016 0.011 39.35 12.57 4.0000 14.92 23.95 0.018 0.012 39.95 12.43 14.75 23.55 0.020 0.012 39.98 12.84 
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表 2 电热板溶解法中不同固液比主要成分的测定结果
Table 2. Measurement results of main components pretreated with electric heating plate dissolution method under different solid-liquid ratios
溶解加水量
(mL)样品C中主要成分的测定值(%) K+ Na+ Ca2+ Mg2+ Cl− SO4 2− 50
75
100
20016.75
16.98
16.64
16.7926.73
27.04
26.85
26.930.024
0.026
0.023
0.0220.006
0.006
0.005
0.00454.25
54.07
54.12
53.850.083
0.081
0.075
0.077
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表 3 电热板溶解方法中不同溶解温度和溶解时间下主要成分的测定结果
Table 3. Measurement results of main components pretreated with electric heating plate dissolution method under different dissolution temperatures and dissolution time
实验样品 溶解温度
(℃)不同溶解温度下主要成分的测定值(%) 溶解时间
(min)不同溶解时间下主要成分的测定值(%) K+ Na+ Ca2+ Mg2+ Cl− SO4 2− K+ Na+ Ca2+ Mg2+ Cl− SO4 2− 样品A 180 10.91 27.06 0.013 0.014 45.91 4.95 10
20
3010.52 27.42 0.014 0.013 45.67 4.71 160 10.53 27.13 0.015 0.014 45.56 4.70 11.05 27.28 0.015 0.014 45.90 4.39 140 10.45 27.27 0.017 0.017 45.08 4.62 10.71 27.31 0.017 0.012 46.13 4.65 样品B 180 14.74 23.55 0.020 0.012 39.63 12.32 10
20
3014.36 23.72 0.018 0.010 39.78 12.39 160 14.32 23.79 0.019 0.012 40.02 12.76 14.81 23.52 0.020 0.013 39.16 12.56 140 14.51 23.41 0.017 0.011 39.29 12.40 14.44 23.32 0.017 0.011 39.93 12.82
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表 4 电热板溶解方法不同搅拌条件下主要成分的测定结果
Table 4. Measurement results of main components pretreated with electric heating plate dissolution method under different stirring conditions
实验样品 搅拌间隔时间
（min）样品中主要成分的测定值(%) K+ Na+ Ca2+ Mg2+ Cl− SO4 2− 样品A 10 10.72 27.23 0.015 0.014 45.43 4.89 5 10.50 27.32 0.016 0.013 45.91 4.66 2 10.41 27.58 0.013 0.013 45.36 4.61 样品B 10 14.20 23.45 0.016 0.010 39.85 12.57 5 14.42 23.61 0.019 0.012 39.66 12.41 2 14.57 23.29 0.018 0.010 39.39 12.85
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表 5 超声振荡溶解方法中不同超声时间和超声功率下主要成分的测定结果
Table 5. Measurement results of main components pretreated with ultrasonic oscillation dissolution method under different ultrasonic time and ultrasonic power
实验样品 超声功率
(Hz)超声时间
(min)样品中主要成分的测定值(%) K+ Na+ Ca2+ Mg2+ Cl− SO4 2− 样品A 60 20
40
6010.79
10.82
10.7527.32
27.51
27.570.014
0.016
0.0170.013
0.014
0.01245.58
46.03
45.374.70
4.33
4.42样品B 60 20
40
6014.86
14.68
14.7523.90
23.49
23.560.017
0.019
0.0200.010
0.011
0.01239.65
39.92
39.2312.75
12.47
12.62样品A 40 20
40
6010.74
10.86
10.8027.58
27.29
27.280.016
0.014
0.0120.013
0.014
0.01345.88
45.52
45.414.58
4.87
4.62样品B 40 20
40
6014.60
14.41
14.4723.74
23.84
23.620.017
0.018
0.0200.013
0.011
0.01039.90
39.55
39.3912.47
12.32
12.66
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表 6 方法检出限
Table 6. Detection limit of the method
组分 测定波长
(nm)方法检出限(µg/g) 电热板溶解法 超声振荡溶解法 K+ 766.490 0.02 0.02 Na+ 330.237 0.01 0.02 Ca2+ 317.933 0.01 0.02 Mg2+ 279.077 0.02 0.02 Cl− / 0.05 0.05 SO4 2− / 0.05 0.05
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表 7 方法精密度和加标回收率
Table 7. Precision and spiked recovery rate of the method
实验样品 分析方法 组分 测定值
(%)加标量
(%)测得总量
(%)RSD
(%)回收率
(%)样品D 电热板溶解法 K+ 8.34 5.00 13.13 2.25 95.80 Na+ 11.08 10.0 20.80 1.80 97.20 Ca2+ 0.026 0.050 0.074 3.19 96.61 Mg2+ 6.61 5.00 11.66 1.82 101.0 Cl− 32.76 25.0 58.24 0.92 101.9 SO4 2− 17.19 10.0 26.98 0.85 97.90 超声振荡
溶解法K+ 8.32 5.00 13.18 1.39 97.20 Na+ 10.94 10.0 20.90 1.19 99.55 Ca2+ 0.025 0.050 0.076 2.96 102.0 Mg2+ 6.56 5.00 11.47 1.43 98.20 Cl− 33.04 25.0 57.67 1.68 98.52 SO4 2− 17.36 10.0 26.89 0.74 95.30 样品E 电热板溶解法 K+ 11.44 5.00 16.30 0.94 97.20 Na+ 6.94 10.0 16.51 1.62 95.70 Ca2+ 0.031 0.050 0.079 2.78 96.00 Mg2+ 6.84 5.00 11.62 1.26 95.62 Cl− 41.68 25.0 66.37 0.52 98.76 SO4 2− 0.823 1.00 1.79 1.14 96.70 超声振荡
溶解法K+ 11.23 5.00 16.0 1.63 95.80 Na+ 6.83 5.00 12.02 1.28 103.8 Ca2+ 0.031 0.050 0.081 3.07 100.4 Mg2+ 6.96 5.00 11.78 1.64 96.40 Cl− 41.63 25.0 66.08 0.55 97.80 SO4 2− 0.804 1.00 1.78 1.42 97.60
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表 8 本文方法与经典分析方法测定结果比对
Table 8. Comparison of measurement results of main components by this method and classical methods
组分 分析方法 样品A
（%）样品B
（%）样品C
（%）样品D
（%）样品E
（%）K+ 电热板溶解法 10.49 14.85 16.85 8.32 11.23 超声振荡溶解法 10.75 14.70 16.98 8.49 11.44 AAS法 11.45 14.31 16.17 8.59 11.62 Na+ 电热板溶解法 27.07 23.93 27.04 10.94 6.94 超声振荡溶解法 27.23 23.67 26.89 11.08 6.77 AAS法 26.05 23.05 26.13 11.22 6.59 Ca2+ 电热板溶解法 0.014 0.016 0.026 0.025 0.031 超声振荡溶解法 0.016 0.018 0.025 0.026 0.032 EDTA容量法 0.016 0.018 0.023 0.029 0.035 Mg2+ 电热板溶解法 0.013 0.011 0.006 6.56 6.84 超声振荡溶解法 0.014 0.012 0.006 6.61 6.96 EDTA容量法 0.015 0.014 0.005 6.73 6.71 Cl− 电热板溶解法 45.55 39.71 54.07 33.04 41.63 超声振荡溶解法 45.91 39.53 53.88 32.76 41.68 硝酸银容量法 45.35 39.15 53.68 33.23 42.05 SO4 2− 电热板溶解法 4.69 12.24 0.083 17.19 0.80 超声振荡溶解法 4.58 12.39 0.081 17.26 0.83 重量法 4.88 12.05 0.089 17.64 0.85
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表 9 样品主要成分百分含量等相关信息
Table 9. Relevant information such as the percentage content of the main components in samples
参数 样品A 样品B 样品C 样品D 样品E 电热板
溶解法超声振荡
溶解法电热板
溶解法超声振荡
溶解法电热板
溶解法超声振荡
溶解法电热板
溶解法超声振荡
溶解法电热板
溶解法超声振荡
溶解法K+ (%) 10.49 10.75 14.85 14.70 16.85 16.98 8.33 8.49 11.23 11.44 Na+ (%) 27.07 27.23 23.93 23.67 27.04 26.89 10.94 11.08 6.94 6.77 Ca2+ (%) 0.014 0.016 0.016 0.018 0.026 0.025 0.025 0.026 0.031 0.032 Mg2+ (%) 0.013 0.014 0.011 0.012 0.006 0.006 6.56 6.61 6.84 6.96 Cl− (%) 45.55 45.91 39.71 39.53 54.07 53.88 33.04 32.76 41.68 41.63 SO4 2− (%) 4.69 4.58 12.24 12.39 0.083 0.081 17.19 17.36 0.823 0.804 HCO3− (%) 0.074 0.072 0.045 0.042 0.005 0.004 0.009 0.008 0.012 0.012 CO32− (%) 0.088 0.085 0.171 0.168 0.001 0.001 / / / / H2O− (%) 4.95 4.76 3.74 3.85 1.16 1.03 4.80 4.91 7.13 7.23 水不溶物(%) 5.82 5.67 4.19 4.37 0.54 0.43 4.18 4.02 3.60 3.76 总水分(%) 5.20 5.05 4.07 4.17 1.18 1.08 18.83 18.92 28.02 28.08 加和方式1(%) 98.76 99.09 98.90 98.75 99.78 99.33 85.07 85.26 78.29 78.63 加和方式2(%) 99.01 99.38 99.23 99.07 99.80 99.38 99.10 99.27 99.18 99.48 B3+ (%) 0.51 0.49 0.78 0.76 / / 0.020 0.021 0.012 0.012 Li+ (%) / / / / / / 0.016 0.016 0.010 0.011 阳离子(mmol/g) 1.45 1.46 1.42 1.41 1.61 1.61 1.23 1.24 1.15 1.16 阴离子(mmol/g) 1.38 1.39 1.38 1.37 1.53 1.52 1.29 1.29 1.19 1.19 R/(+/−)(%) 2.30 2.49 1.71 1.25 2.63 2.71 -2.39 -1.64 -1.67 -1.27 pH 9.50 9.51 9.97 9.98 9.02 9.03 7.93 7.94 7.47 7.46
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