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HACH仪器总磷测定方法

Phosphorus, Total Page 1 of 6
Phosphorus, Total
采样和储存 精度检查
Collect samples in plastic or glass bottles that have been acid washed with 1:1 Hydrochloric Acid Solution (Cat. No. 884‐49) and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning the glassware used in this test. Analyze samples immediately after collection for best results. If prompt analysis is impossible, preserve samples up to 28 days by adjusting the pH to 2 or less with concentrated Sulfuric Acid (about 2 mL per liter) (Cat. No. 979‐49) and storing at 4 °C. Warm the sample to room temperature and neutralize with 5.0 N Sodium Hydroxide (Cat. No. 2450‐53) before analysis. Correct for volume additions; see Section 3.1.3 Correcting for Volume Additions on page 31.
方法 10127
Hach Programs
1. 打开COD的反应堆。
加热至 150 °C. 盖上安全面板
.
2. 触摸
Hach Programs. 使用程序
541 P Total HR ® 吸管
吸取 5.0 mL 去离子水到
总磷 Test ‘N Tube 样品瓶(空白).
4. 使用 TenSette 吸管
吸取 5.0 mL 样品到
总磷Test ‘N Tube 样品瓶 (样品).
福光水务 林琼(译)
Phosphorus, Total Page 1 of 6
总磷
5. 使用漏斗添加膦酸盐‐ 6. 放置样品瓶到 COD
过硫酸钾粉包到每一个样 反应器. 品瓶。. 盖紧帽子和摇动使其溶解.
7. 触摸定时器图标.
触摸 OK. 30分钟的倒计时开始.
8. 计时器发出蜂鸣声后,
请小心地从反应器中的热
瓶. 放置在试管架上,然后
冷却到室温(18–25 °C).
9. 使用TenSette 吸管
添加 2.0 mL 的1.54 N 氢氧化钠 到每一个样品 瓶.
盖上帽子和反转使其混
合.
10. 使用聚乙烯滴管
到样品定位器。 结果将会以 mg/L PO43–.显示
干扰
干扰物

铁 钼 硅 极端 pH或高缓冲样品 氟,钍,铋,硫代硫酸 盐或硫氰酸温度
Large amounts of sample turbidity may cause inconsistent results in the test because the acid present in the reagents may dissolve some of the suspended particles and because of variable desorption of orthophosphate from the particles. The following may interfere when present in concentrations exceeding these listed below:
福光水务 林琼(译)
PhosphorusTot_TNT_High_MOL_Eng_Ody.fm
Phosphorus, Total Page 1 of 6
总磷
Zero
13. 当计时器发出蜂鸣
声, 放置空白瓶到 样品定位器.
14. 触摸 Zero.
界面上显示: 0.0 mg/L PO43–
15. 放入制备好样品瓶
Ba2+, Sr2+, Li+, Na+, K+, NH4+, Cd2+, Mn2+, NO3–, NO2–, SO42–, SO32–, Pb2+, Hg +, Hg2+, Sn2+, Cu2+, Ni2+ , Ag+, U4+ , Zr4+, AsO3–, Br–, CO32–, ClO4–, CN–, IO3–, SiO44–.
提示和技巧
• 使用COD快速消解器的安全面板措施,如果发生飞溅,以防止受伤. •试剂空白,可多次使用,但不得使用超过一天。. •最后的样品将含有钼。此外,最终的样本将有一个小于2 pH值,被认为是由联邦RCRA的腐蚀性(D002)。查阅材料安全数据表数 据的特定信息使用的试剂。
Test ‘N Tube
添加 0.5 mL 的 Molybdovanadate 试剂到每一个样品瓶.
盖上帽子和反转使其
混合.
11. 触摸定时器图标.
触摸 OK. 开始7分钟反应期.
在添加 Molybdovanadate 试剂 后7~9分钟之内读数。
12. 擦拭小瓶用湿毛巾,一
个接着一个干,除去指纹或 其他标识。
Phosphorus, Total Page 2 of 6
DR/2500
方法 10127
Test ‘N Tube™ Vials
应用范围: 应用于水和废水
* 改编自 Standard Methods for the Examination of Water and Wastewater.
总磷
Molybdovanadate 方法 酸性过硫酸消解*
HR (1.0 to 100.0mg/L PO43–)
Standard Additions Method (Sample Spike) 1. Clean glassware with 1:1 Hydrochloric Acid Standard Solution. Rinse again
with deionized water. Do not use detergents containing phosphate to clean glassware. 2. After reading test results, leave the sample cell (unspiked sample) in the instrument. Verify the chemical form. 3. Touch Options. Touch Standard Additions. A summary of the standard additions procedure will appear. 4. Touch OK to accept the default values for standard concentration, sample volume, and spike volumes. Touch Edit to change these values. After values are accepted, the unspiked sample reading will appear in the top row. See Standard Additions in the DR/2500 instrument manual for more information. 5. Snap the neck off a 10‐mL Voluette® Ampule of Phosphate Standard Solution, 500 mg/L as PO43–. 6. Prepare three sample spikes. Fill three mixing cylinders (Cat. No. 1896‐40) with 10 mL of sample. Use the TenSette Pipet to add 0.1 mL, 0.2 mL, and 0.3 mL of standard, respectively to each cylinder. Mix well. 7. Analyze each sample spike as described in the procedure above, starting with the 0.1 mL sample spike. Accept each standard additions reading by touching Read. Each addition should reflect approximately 100% recovery or an increase of 5 mg/L PO43– for each 0.1 mL of standard added. 8. After completing the sequence, touch Graph to view the best‐fit line through the standard additions data points, accounting for matrix interferences. Touch View: Fit, then select Ideal Line and touch OK to view the relationship between the sample spikes and the “Ideal Line” of 100% recovery. See Section 3.2.2 Standard Additions on page 36 for more information.
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