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【讨论帖】是纯水污染还是?
请分析:【讨论帖】是纯水污染还是?
1.走超纯水也有微量的氯和溴,但是有溴的纯水谱图,一般是在积分项下选“建议”框后才出现,有时做样品时其实也是一样的,不选择“建议”项,就不积分出微量的溴。会不会是由于噪音影响基线的波动而出现并不能算做溴峰的波浪,而被仪器认定为溴呢?
2.做了四个超纯水的样,纯水1、2、3三个图都有出现氯和溴,只有一个谱图(第3个图)没有,但是这个是在基线(开机后只走了20多分钟才进的)未走稳时走的,特别是后面两个是连续走的,应该可以排除做完样品后残留 的氯的干扰.是超纯水污染还是和第一个我怀疑的一样的原因呢?
3,第2个图谱是做的空白,就是同样燃烧脱脂棉,用吸收液吸收,过滤纸到容量瓶。和做样相比,只是没有样品的参与。综合以上出现的问题,请问这个空白值可信度高不?实验是成功的不?
为谢!
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【讨论帖】是纯水污染还是?
【讨论帖】是纯水污染还是?
最新回复
xuuuu (2015-11-18 14:35:10)
纯水2图谱
Printed by: 761 ic
Ident: up-water-1224-2
Analysis from: 2009-12-24 11:13:40
File: tc241113.chw Last save: 2009-12-24 11:31:38
Method: ASUPP4_250.mtw Last save: 2009-12-24 9:52:58
Run operator: 761 ic
Analysis number: 271
SAMPLE:
:
Vial number: 0
Volume: 20.0 礚
Dilution: 1.00
Amount: 1.0000
COLUMN: METROSEP A SUPP 4 - 250 (6.1006.430)
Size: 4.0 x 250 mm
Number:
Part.size: 9.0 祄
ELUENT: 1.8 mmol/l Na2CO3 / 1.7 mmol/L NaHCO3
Flow: 1.00 mL/min
Temperature: 20.0癈
Pressure: 9.1 MPa
0
[ 本帖最后由 xuuuu 于 2015-11-18 14:37 编辑 ]
2009122414275.jpg
xuuuu (2015-11-18 14:37:55)
Report date: 2009-12-24 13:45:56
Printed by: 761 ic
Ident: 空白
Analysis from: 2009-12-24 10:47:00
File: tc241047.chw Last save: 2009-12-24 11:04:58
Method: ASUPP4_250.mtw Last save: 2009-12-24 9:52:58
Run operator: 761 ic
Analysis number: 270
SAMPLE:
:
Vial number: 0
Volume: 20.0 礚
Dilution: 1.00
Amount: 1.0000
COLUMN: METROSEP A SUPP 4 - 250 (6.1006.430)
Size: 4.0 x 250 mm
Number:
Part.size: 9.0 祄
ELUENT: 1.8 mmol/l Na2CO3 / 1.7 mmol/L NaHCO3
Flow: 1.00 mL/min
Temperature: 20.0癈
Pressure: 8.7 MPa
Quantitation method: Custom
No Retention Height Area Conc. Name
min uS/cm uS/cm*sec mg/L
1 3.93 0.05 0.731 0.089 F
2 5.05 0.07 2.473 0.000
3 5.41 0.11 1.552 0.191 Cl
4 6.07 0.47 8.099 0.000
5 7.48 0.00 0.025 0.099 Br
6 8.29 1.12 25.583 0.000
7 10.07 0.10 3.764 0.000
8 12.57 0.00 0.009 0.000
9 13.39 0.00 0.005 0.000
Page 2; tc241047.chw; 24/12/2009 13:45:56
10 15.10 0.11 4.581 0.000
11 16.87 0.00 0.179 0.000
_____________________________________________
11 18.00 2.04 47.000 0.379
This report has been created by IC Net
METROHM LTD
20091224144728.jpg
xuuuu (2015-11-18 14:38:16)
Report date: 2009-12-24 13:39:54
Printed by: 761 ic
Ident: UP-WATER-2-1224
Analysis from: 2009-12-24 8:57:54
File: tc240857.chw Last save: 2009-12-24 9:15:52
Method: ASUPP4_250.mtw Last save: 2009-12-24 8:50:10
Run operator: 761 ic
Analysis number: 265
SAMPLE:
:
Vial number: 0
Volume: 20.0 礚
Dilution: 1.00
Amount: 1.0000
COLUMN: METROSEP A SUPP 4 - 250 (6.1006.430)
Size: 4.0 x 250 mm
Number:
Part.size: 9.0 祄
ELUENT: 1.8 mmol/l Na2CO3 / 1.7 mmol/L NaHCO3
Flow: 1.00 mL/min
Temperature: 20.0癈
Pressure: 9.8 MPa
Quantitation method: Custom
No Retention Height Area Conc. Name
min uS/cm uS/cm*sec mg/L
1 4.12 0.03 0.736 0.000
This report has been created by IC Net
METROHM LTD
2009122414502.jpg
xuuuu (2015-11-18 14:38:35)
Printed by: 761 ic
Ident: up-1224-2
Analysis from: 2009-12-24 10:25:05
File: tc241025.chw Last save: 2009-12-24 13:43:46
Method: ASUPP4_250.mtw Last save: 2009-12-24 9:52:58
Run operator: 761 ic
Analysis number: 269
SAMPLE:
:
Vial number: 0
Volume: 20.0 礚
Dilution: 1.00
Amount: 1.0000
COLUMN: METROSEP A SUPP 4 - 250 (6.1006.430)
Size: 4.0 x 250 mm
Number:
Part.size: 9.0 祄
ELUENT: 1.8 mmol/l Na2CO3 / 1.7 mmol/L NaHCO3
Flow: 1.00 mL/min
Temperature: 20.0癈
Pressure: 8.9 MPa
Quantitation method: Custom
No Retention Height Area Conc. Name
min uS/cm uS/cm*sec mg/L
1 4.06 0.02 0.920 0.000
2 4.96 0.01 0.239 0.000
3 5.55 0.01 0.276 0.092 Cl
4 7.56 0.00 0.033 0.101 Br
5 8.25 0.01 0.168 0.000
6 9.57 0.00 0.045 0.000
7 10.33 0.00 0.070 0.000
8 11.25 0.00 0.004 0.000
9 11.67 0.00 0.002 0.000
Page 2; tc241025.chw; 24/12/2009 13:44:30
10 12.13 0.00 0.020 0.000
11 14.36 0.00 0.017 0.000
12 15.16 0.00 0.099 0.000
13 16.95 0.00 0.026 0.000
14 17.71 0.00 0.001 0.000
_____________________________________________
14 18.00 0.05 1.920 0.193
This report has been created by IC Net
METROHM LTD
20091224145426.jpg
xuuuu (2015-11-18 14:39:33)
Report date: 2009-12-24 13:45:31
Printed by: 761 ic
Ident: up-water-1224-3
Analysis from: 2009-12-24 11:38:30
File: tc241138.chw Last save: 2009-12-24 11:56:28
Modified!
Method: ASUPP4_250.mtw Last save: 2009-12-24 9:52:58
Run operator: 761 ic
Analysis number: 272
SAMPLE:
:
Vial number: 0
Volume: 20.0 礚
Dilution: 1.00
Amount: 1.0000
COLUMN: METROSEP A SUPP 4 - 250 (6.1006.430)
Size: 4.0 x 250 mm
Number:
Part.size: 9.0 祄
ELUENT: 1.8 mmol/l Na2CO3 / 1.7 mmol/L NaHCO3
Flow: 1.00 mL/min
Temperature: 20.0癈
Pressure: 8.6 MPa
Quantitation method: Custom
No Retention Height Area Conc. Name
min uS/cm uS/cm*sec mg/L
1 4.05 0.02 1.161 0.000
2 4.78 0.01 0.223 0.000
3 5.22 0.01 0.077 0.077 Cl
4 5.92 0.00 0.048 0.000
5 6.85 0.00 0.151 0.000
6 8.71 0.00 0.007 0.000
7 9.53 0.00 0.012 0.000
8 10.35 0.00 0.165 0.000
9 12.51 0.00 0.105 0.000
Page 2; tc241138.chw; 24/12/2009 13:45:31
10 13.86 0.00 0.061 0.000
11 15.27 0.00 0.129 0.000
12 16.94 0.00 0.038 0.000
_____________________________________________
12 18.00 0.06 2.179 0.077
This report has been created by IC Net
METROHM LTD
2009122414562.jpg
loli (2015-11-18 14:39:54)
1你的纯水可能是稍稍有些问题,有微量的氯残留
2 对于某些特殊的色谱图,需要调整积分参数,但“建议”并不是很好的选择,显然那个被系统误认为是Br 的峰很不规则。
3 你的燃烧脱脂棉的空白谱图中NO2 和NO3 很高,说明氧弹燃烧操作手法上还不够好,充氧不足,N2太多,燃烧不完全。
4 可以平衡再长一点时间进针水看看会不会好些!
ujne (2015-11-18 14:40:49)
1你的纯水可能是稍稍有些问题,有微量的氯残留
2 对于某些特殊的色谱图,需要调整积分参数,但“建议”并不是很好的选择,显然那个被系统误认为是Br 的峰很不规则。
3 你的燃烧脱脂棉的空白谱图中NO2 和NO3 很高,说明氧弹燃烧操作手法上还不够好,充氧不足,N2太多,燃烧不完全。
4 可以平衡再长一点时间进针水看看会不会好些!
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我在检测中用的超纯水也含有少量的F,Cl,硫酸根,但没有更纯的水了。我的机器是ICS2000,用超纯水做淋洗液。
iii_ii (2015-11-18 14:41:36)
我们都没出现这样的问题啊1~!
911 (2015-11-18 14:41:52)
koook5695 (2015-11-18 14:42:15)
qhyu (2015-11-18 14:42:40)
xiaoxiaoniao (2015-11-18 14:42:59)
3.14 (2015-11-18 14:43:21)
cocacola (2015-11-18 14:43:40)
ladyhuahua (2015-11-18 14:43:57)
pore (2015-11-18 14:44:47)
【讨论帖】是纯水污染还是?