印尼庞卡兰苏苏火电项目部

PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

现场操作培训记录卡
On-site Operation Training Record Card

培训项目
铁的测定
Training project

Determination of Fe
培训日期 2019.02.21 培训老师
Training Date Trainer
巡回检查的内容和标准(Contents and standards of patrol inspection)：

铁的测定
Determination of Fe
(邻菲罗啉分光光度法 o-phenanthroline spectrophotometry）
1 概 要 Summary
1.1 先将高铁用盐酸羟胺还原成亚铁。在 pH 为 4～5 的条件下，亚铁与
邻菲罗啉生成浅红色络合物，此络合物的最大吸收波长为 510nm。
1.1 Firstly, reduce high-iron to ferrous iron by using hydroxylamine
hydrochloride. At a PH value of 4 to 5, the ferrous iron and o-
phenanthroline can form a light red complex, and the maximum
absorption wavelength of the complex is 510nm.
1.2 本法的测定范围为 5～200μg/L，测得的结果为水样的全铁量。
1.2 The measurement range of this method is 5 ～ 200μg/L, the measured
result is the total iron content of the water sample.
2 仪器
2 Instruments
2.1 50ml 容量瓶
2.1 50ml measuring flask
2.2 100ml 或 150ml 锥形瓶
2.2 100ml or150ml conical beaker
2.3 751 型分光光度计：本计附有 100mm 比色皿
 印尼庞卡兰苏苏火电项目部
PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

2.3 751 type spectrophotometer: this meter is equipped with 100mm cuvette
3 试剂
3 Reagents
3.1 10%盐酸羟胺溶液（重/容）： 称取 10g 盐酸羟胺(NH2OH·HCl)，
加入少高纯水，待溶解后用高纯水稀释至 100ml，摇匀并贮于棕
色瓶中，塞紧瓶塞。
3.1 10% hydroxylamine hydrochloride solution (weight/capacity): weigh
10g of hydroxylamine hydrochloride (NH2OH·HCl), add a small
amount of high purity water, and dilute it to 100ml after dissolution.
Shake it to make it well dissolved, and store it in a brown bottle, and
well stuff the stopper.
3.2 0.1%邻菲罗啉溶液（重/容）： 称取 1g 邻菲罗啉（C12H8N2.H2O）
溶于 100ml 无水乙醇中，用高纯水稀释至 1L，摇匀，贮于棕色瓶
中，并在暗处保存。
3.2 0.1% o-phenanthroline solution (weight/capacity): weigh 1g of o-
phenanthroline（C12H8N2.H2O）and dissolve it in 100ml absolute
ethanol, dilute it to 1L with high purity water, shake to well dissolved,
and store it in a brown bottle, and in a dark place.
3.3 乙酸---乙酸铵缓冲液： 称取 100g 乙酸铵（CH3COONH4）溶于
100ml 高纯水中，加入 200ml 冰乙酸（CH3COOH），用高纯水稀
释至 1L，摇匀后贮存。
3.3 Acetic acid---ammonium acetate buffer solution: weigh 100g of
ammonium acetate (CH3COONH4) and dissolve it in 100ml of high
purity water, add 200ml of glacial acetic acid (CH3COOH), dilute it to
1L by using high purity water. Store it after well shaking.
3.4 铁贮备溶液（1ml 含 100μgFe）： 称取 0.1000g 纯铁丝，加入
1mol/L 盐酸溶液 50mL，加热全部溶解后，加入少量过硫酸铵，煮
沸数分钟，移入 1L 容量瓶中，用高纯水稀释至刻度。或者称取
0.8634g 硫酸高铁铵［NH4Fe(SO4)2.12H2O］，溶于 50mL 1mol/L 盐
酸溶液中，全部溶解后移入 1L 容量瓶中，用高纯水稀释至刻度，
用重量法标定其浓度。
3.4 Iron backup solution (1ml containing 100μgFe): weigh 0.1000g pure
iron wire, add 50ml of 1mol/L hydrochloric acid solution, heat it until
completely dissolved, add as small amount of ammonium persulfate,
boil for a few minutes, transfer it to a 1L measuring flask, and dilute to
the mark with high purity water.
 印尼庞卡兰苏苏火电项目部
PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

Or weigh 0.8634g of ammonium ferric sulfate [NH4Fe(SO4)2.12H2O],

dissolve it in 50ml of 1mol/L hydrochloric acid solution, transfer it to a
1L measuring flask after well dissolved, dilute it to the mark with high
purity water. Calibrate its concentration by gravimetric determination
method.
3.5 铁工作溶液（1ml 含 1μgFe）： 移取铁贮备溶液（1ml 含
100μgFe）10.00ml，注入 1L 容量瓶中，加入 1mol/L 盐酸溶液
10mL，用高纯水稀释至刻度（此溶液使用时配制）。
3.5 Iron working solution (1ml containing 1μgFe): take 10.00ml of iron
backup solution (1ml containing 100μgFe), inject into a 1L volumetric
flask, add 10ml of 1mol/L hydrochloric acid solution, dilute it to the
mark with high purity water (this solution is prepared when it is going
to be used).
3.6 浓盐酸（优级纯）。
3.6 Concentrated hydrochloric acid (excellent grade).
3.7 浓氨水。
3.7 Concentrated ammonia.
3.7 刚果红试纸：需切成 4mm×4mm 的小方块。
3.7 Congo red test paper: cut into small squares of 4mm×4mm.
4 测定方法
4 Method of Measurement
4.1 工作曲线绘制：
4.1 Working curve drawing:
4.1.1 按表中取铁工作溶液注入一组 50mL 容量瓶中，并用高纯水稀释
至刻度。
4.1.1 Take the iron working solution according to the table, and pour it into a
set of 50mL volumetric flask and dilute it to the scale with high purity
water.
铁标准溶液的配制 Preparation of Iron Standard Solution
 印尼庞卡兰苏苏火电项目部
PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

编 号 No. 0 1 2 3 4 5 6 7 8 9 10 11

取铁工作溶液

Iron working 0 0.5 1.0 2.0 3.0 4.0 5.0 6.0 7.0 8.0 9.0 10.0

solution (mL)

相当于水样含铁量

Iron content in
0 10 20 40 60 80 100 120 140 160 180 200
the water

sample（μg/L）

4.1.2 将配制好的标准溶液分别移入一组编号相对应的 100ml 或 150ml

锥形瓶或同样容积的烧杯中，各加入 1ml 浓盐酸，加热浓缩至体
积略小于 25ml。冷却至 30℃左右，加入 1ml 盐酸羟胺溶液，摇
匀，静置 5min，加入 5ml 0.1%邻菲罗啉溶液，摇匀后每个锥形瓶
中各加入一小块刚果红试纸，慢慢滴加氨水调节 pH 至 3.8～4.1，
使刚果红试纸恰由蓝色转变为紫色【为了避免氨水在调整过程中

过量（即刚果红试纸变成红色），一般可先加入 0.8ml 浓氨水，

然后用（1+1）氨水逐滴调节】，然后依次加 5ml 乙酸---乙酸铵缓

冲液。摇匀后移入原 50ml 容量瓶中，用高纯水稀释至刻度。在 751
分光光度计上，用波长 510nm，100mm 长比色皿，用高纯水为参
比测定吸光度。
4.1.2 The prepared standard solution is respectively moved into a set of
100ml or 150ml conical flasks or beakers with the same volume with
corresponding number. Add 1ml of concentrated hydrochloric acid,
and the mixture is heated until the volume decreases to slightly less
than 25ml. Cool it to about 30℃, and then dose 1ml of hydroxylamine
hydrochloride solution, wait for 5min after shaking, add 5ml of 0.1%
 印尼庞卡兰苏苏火电项目部
PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

0-phenanthrene solution. Put a small piece of Congo red test paper in

each conical flask. Slowly add ammonia water to adjust the pH to 3.8-
4.1, the Congo red test paper is just changed from blue to purple [in
order to avoid the excess of ammonia water in the adjustment
process (that is, the Congo red test paper becomes red), 0.8ml of
concentrated ammonia water can be added first, and then use
(1+1) ammonia water drop to gradually adjust], and then dose 5ml
of acetic acid, and ammonium acetate buffer solution in sequence.
Move the solution to the 50ml volumetric flask after shaking, and
dilute it to the scale with high purity water. In a 751
spectrophotometer, absorbance was measures with high purity water as
a reference by using a cuvette with a wavelength of 510nm and a
length of 100mm.
4.1.3 将所测吸光度值减去编号为“0”的空白值（包括高纯水和单倍试
剂的空白值）后，和相应的含铁量绘制工作曲线。
4.1.3 After the measured absorbance value is subtracted from the blank
value with No, “0” (including high purity water and single reagent),
and the working curve is drawn according to the corresponding iron
content.
4.2 水样的测定
4.2 Determination of Water Sample
1）将取样瓶用（1+1）盐酸浸泡或煮洗，再用高纯水反复清洗后
使用。然后往取样瓶中加入浓盐酸（每 500mL 水样加浓盐酸
2mL），直接采取水样，取样后即将水样摇匀。
1) Soaking or boiling the sample bottle with (1+1) hydrochloric acid,
and repeatedly cleaning with high purity water, and then the bottle
can be used. Add concentrated hydrochloric acid into the sample
bottle (add 2ml of concentrated hydrochloric acid per 500ml of
water sample), directly take the water sample. Shake the water
sample after sampling.
2）取 50ml 水样于 150ml 锥形瓶或烧杯中，加入 1ml 浓盐酸，加热
浓缩至体积略小于 25ml。冷却至 30℃左右，加入 1ml 盐酸羟胺
溶液，摇匀。静置 5min，加入 5ml 0.1%邻菲罗啉溶液，摇匀后每
个锥形瓶中各加入一小块刚果红试纸，慢慢滴加氨水调节 PH 至
3.8～4.1，使刚果红试纸恰由蓝色转变为紫色，然后依次加入
5ml 乙酸---乙酸铵缓冲液。摇匀后移入 50ml 容量瓶中，用高纯水
稀释刻度。在 751 型分光光度计上，用波长 510nm，100mm 长比
 印尼庞卡兰苏苏火电项目部
PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

色皿，以高纯水参比测定吸光度。
2) Take 50ml of water sample in a 150ml conical flask or beaker, and
then add 1ml of concentrated hydrochloric acid, and the mixture is
heated until the volume decreases to slightly less than 25ml. Cool it
to about 30℃, and then dose 1ml of hydroxylamine hydrochloride
solution, wait for 5min after shaking, add 5ml of 0.1% 0-
phenanthrene solution. Put a small piece of Congo red test paper in
each conical flask. Slowly add ammonia water to adjust the pH to
3.8-4.1, the Congo red test paper is just changed from blue to purple,
and then dose 5ml of acetic acid, and ammonium acetate buffer
solution in sequence. Move the solution to the 50ml volumetric flask
after shaking, and dilute it to the scale with high purity water. In a
751 spectrophotometer, absorbance was measures with high purity
water as a reference by using a cuvette with a wavelength of 510nm
and a length of 100mm.
3）同时作单倍试剂和双倍试剂空白试验，双倍试剂和单倍试剂空白
值之差作为试剂空白值。 即：双倍试剂空白值-单倍试剂空白值

=试剂空白值
3) Do the single reagent and double reagent blank test at the same time,
the difference between the blank values of the double reagent and the
single reagent is used as the reagent blank value. That is, double
reagent blank value – single reagent blank value = reagent blank
value.
4）测得的水样吸光度值扣除试剂空白值后，查工作曲线即得水样中
的含铁量。
4) After the measured water sample absorbance value is subtracted from
the reagent blank value, check the working curve, then you can get
the iron content in the water sample.

样品吸光度（A)在 7230G 分光光度计上的测试

Sample Absorbance (A) Test on 723G Spectrophotometer

1. 按动“功能键”，切换至透射比测试模式。
1. Press “Function”, switch to the %TRANS mode.
2. 旋动仪表正面上的旋钮，调节测试波长为 510nm。
 印尼庞卡兰苏苏火电项目部
PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

2. Adjust the knob in the front of the instrument to adjust the testing wavelength to
be 510nm.
3. 打开比色室盖，放入黑色遮光体，盖上比色室盖，推动拉杆使遮光体处于
光路中，按动“调 0%T”键，此时仪器显示“00.0”或“-00.0”。
3. Open the sample compartment, and put the black occulter in it, and then close
the sample compartment. Use the pull rod to make sure that the occulter is in
the beam path. Press “Adjust 0%T”, at this time, the instrument will read
“00.0” or “-00.0”.
4. 按动“功能键”，切换至吸光度测试模式。
4. Press “Function”, switch to the absorbance test mode.
5. 将清洗干净的两只 10mm 比色皿倒入高纯水，擦干水后放入比色池，盖上
盖子，推动拉杆先使一只比色皿处于光路中，按动“100%T”键，此时仪
器显示“BL”数秒后显示“-.000”或“.000”，推动拉杆使另一只比色皿处
于光路中，仪器也应显示“-.000”或“.000”，否则，应重新选取两只透光
完全一样的比色皿。
5. Take 2 clean 10mm cuvettes, add high purity water. After they are dried, put it
into the cuvette rack, and then cover it. Push the pull rod to make one cuvette in
the beam path, press “100%T”, at this time, the instrument reads “BL”, after
several seconds later, it reads “-.000” or “.000”. Then push the pull rod to make
sure the other cuvette is in the beam path, the instrument shall reads “-.000” or
“.000”. Otherwise, two cuvettes with exactly same light-transmitting shall be
re-selected.
6. 取出一只比色皿，倒入待测水样，擦干水后放入比色池，盖上盖子，推动
拉杆先使其处于光路中，仪表显示的数值就是水样的吸光度值。
6. Take out one cuvette, and add the water sample to be tested. After it is dried,
put it in the cuvette rack. Close the cover. Push the pull rod to make it in the
beam path. The reading on the instrument display is the absorbance of the water
sample value.
 印尼庞卡兰苏苏火电项目部
PANGK ALAN SUSU COAL FIRED STEA M POWER PLANT PROJECT UNIT
3&4 2X200MW

培训签到
SIGNATURE