China's Refractories ›› 2020, Vol. 29 ›› Issue (2): 37-41.DOI: 10.19691/j.cnki.1004-4493.2020.02.007
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WANG Yanni, HAN Dan, LEI Xiaoyu, ZHANG Yajing
Revised:2021-05-13
Online:2020-06-15
Published:2020-06-15
About author:Wang Yanni, born in 1986, gained her bachelor's degree from Zhengzhou University in 2009 and master's degree from University of Science and Technology Beijing in 2012, majored in material science and technology. Since then, she has been working in Sinosteel Luoyang Institute of Refractories Research Co., Ltd.
WANG Yanni, HAN Dan, LEI Xiaoyu, ZHANG Yajing. Determination of Boron in Refractories[J]. China's Refractories, 2020, 29(2): 37-41.
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URL: http://www.cnref.cn/EN/10.19691/j.cnki.1004-4493.2020.02.007
| Methods | Recovered B2O3 /mg | Average value /mg | Relative standard deviation (n=6) /% |
|---|---|---|---|
| Method 1 | 9.96, 9.95, 9.99, 9.98, 9.96, 9.98 | 9.97 | 0.16 |
| Method 2 | 9.97, 9.96, 9.95, 9.98, 9.97, 9.95 | 9.96 | 0.12 |
Table 1 Comparison of end point determination by two methods
| Methods | Recovered B2O3 /mg | Average value /mg | Relative standard deviation (n=6) /% |
|---|---|---|---|
| Method 1 | 9.96, 9.95, 9.99, 9.98, 9.96, 9.98 | 9.97 | 0.16 |
| Method 2 | 9.97, 9.96, 9.95, 9.98, 9.97, 9.95 | 9.96 | 0.12 |
| Reference materials | Measured value /% | Average value /% | Certified value /% | Relative standard deviation (n=6) /% |
|---|---|---|---|---|
| BCS372 | 2.36, 2.34, 2.35, 2.35, 2.34, 2.32 | 2.34 | 2.35 | 0.58 |
| YSB1674-05 | 5.70, 5.68, 5.71, 5.69, 5.70, 5.66 | 5.69 | 5.65 | 0.31 |
| GBW03132 | 8.87, 8.80, 8.81, 8.84, 8.88, 8.86 | 8.84 | 8.87 | 0.37 |
Table 2 Precision and accuracy tests by alkaline titrimetry
| Reference materials | Measured value /% | Average value /% | Certified value /% | Relative standard deviation (n=6) /% |
|---|---|---|---|---|
| BCS372 | 2.36, 2.34, 2.35, 2.35, 2.34, 2.32 | 2.34 | 2.35 | 0.58 |
| YSB1674-05 | 5.70, 5.68, 5.71, 5.69, 5.70, 5.66 | 5.69 | 5.65 | 0.31 |
| GBW03132 | 8.87, 8.80, 8.81, 8.84, 8.88, 8.86 | 8.84 | 8.87 | 0.37 |
| Reference materials | Measured value /mass% | Average value /mass% | Certified value /mass% | Relative standard deviation (n=6) /% |
|---|---|---|---|---|
| BCS389 | 0.027, 0.029, 0.029, 0.028, 0.027, 0.026 | 0.028 | 0.029 | 4.38 |
| BCS396 | 0.089, 0.092, 0.090, 0.091, 0.088, 0.090 | 0.090 | 0.09 | 1.57 |
| JRRM301 | 0.82, 0.84, 0.89, 0.90, 0.91, 0.87 | 0.87 | 0.87 | 4.07 |
| BCS372 | 2.30, 2.28, 2.38, 2.31, 2.34, 2.40 | 2.34 | 2.35 | 2.02 |
| GBW03132 | 8.76, 8.81, 8.90, 8.84, 8.85, 8.79 | 8.82 | 8.87 | 0.56 |
Table 3 Precision and accuracy tests by ICP-AES
| Reference materials | Measured value /mass% | Average value /mass% | Certified value /mass% | Relative standard deviation (n=6) /% |
|---|---|---|---|---|
| BCS389 | 0.027, 0.029, 0.029, 0.028, 0.027, 0.026 | 0.028 | 0.029 | 4.38 |
| BCS396 | 0.089, 0.092, 0.090, 0.091, 0.088, 0.090 | 0.090 | 0.09 | 1.57 |
| JRRM301 | 0.82, 0.84, 0.89, 0.90, 0.91, 0.87 | 0.87 | 0.87 | 4.07 |
| BCS372 | 2.30, 2.28, 2.38, 2.31, 2.34, 2.40 | 2.34 | 2.35 | 2.02 |
| GBW03132 | 8.76, 8.81, 8.90, 8.84, 8.85, 8.79 | 8.82 | 8.87 | 0.56 |
| Temperature /℃ | 30 | 40 | 50 | 52 | 55 | 58 | 60 | 70 |
|---|---|---|---|---|---|---|---|---|
| Absorbance | 0.10 | 0.18 | 0.20 | 0.26 | 0.28 | 0.27 | 0.25 | 0.21 |
Table 4 Effect of water bath temperature on absorbance
| Temperature /℃ | 30 | 40 | 50 | 52 | 55 | 58 | 60 | 70 |
|---|---|---|---|---|---|---|---|---|
| Absorbance | 0.10 | 0.18 | 0.20 | 0.26 | 0.28 | 0.27 | 0.25 | 0.21 |
| Holding time /min | 0 | 10 | 20 | 30 | 40 | 50 | 60 |
|---|---|---|---|---|---|---|---|
| Absorbance | 0.214 | 0.262 | 0.340 | 0.342 | 0.347 | 0.344 | 0.345 |
Table 5 Effect of holding time after evaporation to dryness
| Holding time /min | 0 | 10 | 20 | 30 | 40 | 50 | 60 |
|---|---|---|---|---|---|---|---|
| Absorbance | 0.214 | 0.262 | 0.340 | 0.342 | 0.347 | 0.344 | 0.345 |
| m (B2O3) /μg | 0 | 1 | 2 | 3 | 4 | 5 | |
|---|---|---|---|---|---|---|---|
| Absorbance | 100 mL dish | 0.125 | 0.181 | 0.223 | 0.270 | 0.296 | 0.340 |
| 250 mL dish | 0.094 | 0.389 | 0.438 | 0.514 | 0.552 | 0.671 | |
Table 6 Effect of evaporation rate on absorbance
| m (B2O3) /μg | 0 | 1 | 2 | 3 | 4 | 5 | |
|---|---|---|---|---|---|---|---|
| Absorbance | 100 mL dish | 0.125 | 0.181 | 0.223 | 0.270 | 0.296 | 0.340 |
| 250 mL dish | 0.094 | 0.389 | 0.438 | 0.514 | 0.552 | 0.671 | |
| m (B2O3) /μg | 0 | 1 | 2 | 3 | 4 | 5 | |
|---|---|---|---|---|---|---|---|
| Absorbance | 10 min | 0.063 | 0.234 | 0.379 | 0.489 | 0.482 | 0.589 |
| 30 min | 0.060 | 0.234 | 0.381 | 0.491 | 0.476 | 0.593 | |
| 60 min | 0.062 | 0.233 | 0.380 | 0.491 | 0.481 | 0.592 | |
Table 7 Coloration stability tests
| m (B2O3) /μg | 0 | 1 | 2 | 3 | 4 | 5 | |
|---|---|---|---|---|---|---|---|
| Absorbance | 10 min | 0.063 | 0.234 | 0.379 | 0.489 | 0.482 | 0.589 |
| 30 min | 0.060 | 0.234 | 0.381 | 0.491 | 0.476 | 0.593 | |
| 60 min | 0.062 | 0.233 | 0.380 | 0.491 | 0.481 | 0.592 | |
| m (B2O3) /μg | 0 | 1 | 2 | 3 | 4 | 5 | |
|---|---|---|---|---|---|---|---|
| Absorbance | Batch 1 | 0.037 | 0.189 | 0.241 | 0.291 | 0.482 | 0.589 |
| Batch 2 | 0.071 | 0.220 | 0.285 | 0.345 | 0.501 | 0.629 | |
Table 8 Repeatability tests
| m (B2O3) /μg | 0 | 1 | 2 | 3 | 4 | 5 | |
|---|---|---|---|---|---|---|---|
| Absorbance | Batch 1 | 0.037 | 0.189 | 0.241 | 0.291 | 0.482 | 0.589 |
| Batch 2 | 0.071 | 0.220 | 0.285 | 0.345 | 0.501 | 0.629 | |
| Reference materials | Measured value /mass% | Average value /mass% | Certified value /mass% | Relative standard deviation (n=6) /% |
|---|---|---|---|---|
| BCS389 | 0.024, 0.022, 0.025, 0.022, 0.026, 0.024 | 0.024 | 0.029 | 6.72 |
| BCS396 | 0.089, 0.086, 0.092, 0.090, 0.085, 0.094 | 0.089 | 0.090 | 3.86 |
| JRRM301 | 0.88, 0.86, 0.90, 0.91, 0.86, 0.94 | 0.89 | 0.87 | 3.50 |
Table 9 Precision and accuracy tests by curcumin absorption spectrophotometry
| Reference materials | Measured value /mass% | Average value /mass% | Certified value /mass% | Relative standard deviation (n=6) /% |
|---|---|---|---|---|
| BCS389 | 0.024, 0.022, 0.025, 0.022, 0.026, 0.024 | 0.024 | 0.029 | 6.72 |
| BCS396 | 0.089, 0.086, 0.092, 0.090, 0.085, 0.094 | 0.089 | 0.090 | 3.86 |
| JRRM301 | 0.88, 0.86, 0.90, 0.91, 0.86, 0.94 | 0.89 | 0.87 | 3.50 |
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