Upload
others
View
2
Download
0
Embed Size (px)
Citation preview
It should never be assumed that measurement results arebasically correct; there is always a possibility that they errorsmay have occurred at some stage of the analysis procedure.
In the field of chemical analysis, possible sources of error arethe materials used, the handling routines associated with theanalytical system, and the water samples to be analyzed(matrix influences).
The errors influence the accuracy and precision of the resultsof the measurements.
Accuracy: deviation of the results from the actual con-centration;
Precision: scatter of the results among each other.
Accurate and precise results of measurements are howeverthe prerequisite for:
• complying with and monitoring limiting values• the control of production• conditioning and purification processes.
Moreover, these measurements are used as a basis formaking decisions that often involve large financial expen-diture. As the responsibility for the measurement results liesin principle with the user, he must be certain about thequality of his results.
In the operation analysis sector Dr. Lange has developed anAQA system which is specially tailored to the requirements ofthe user – the 4-pillar concept. This allows the user to achieveaccurate, precise and comparable analytical results.
The basis of this 4-pillar concept is addista .
AnalyticalQuality Assurance (AQA)(The 4-pillar concept)
Assurance with addista
Summary:
Consistent application of the 4 pillars of the analytical quality assurance system provides the user with an effective means ofchecking and monitoring his analysis results.The fundamental advantages for the user are:
• reproducible analysis results• reliable measurement data as an aid to assessment and decision-making• analytical security through recognition of interferences and handling errors
The 4-pillar concept
Control of handling Analysis External check Comparabilityand materials of a water sample for of the measuring system to reference method
interferences and handling
addista Standard solutions Spikings solutions Ring test solutions Ref./cuvette test compara-components bility investigation in the
Dr. Lange standard laboratory
Recommended every 10th sample, every 20th sample, Twice per year Twice per yearminimum frequency at least once per month at least once every 3 month per cuvette test per paramter
(depends on person)
Documentation Standard control card Recovery control card Ring test evaluation Investigation reportwith diploma
Quality AssuranceLCA addista
Data table addista
Edition: 4/02
GB
Test expressed as Standardnominal value max. deviation
mg/l mg/l
Spiking resultnominal value max. deviation
mg/l mg/l
LCA 701 LCK 306LCK 321LCK 329LCK 337LCK 353LCK 360
Pb (II)Fetot.
Cu (II)NiSO4
Zn
0.5 ± 0.13 ± 0.152 ± 0.12 ± 0.1
500 ± 502 ± 0.15
0.25 ± 0.151.5 ± 0.21 ± 0.151 ± 0.15
250 ± 601 ±0.2
LCA 702 LCK 301LCK 308LCK 313
LCK 353
AlCdCr (VI)Crtot.
SO4
0.3 ± 0.020.2 ± 0.030.5 ± 0.050.5 ± 0.05500 ± 50
0.15 ± 0.030.1 ± 0.040.25 ± 0.060.25 ± 0.06250 ± 60
LCA 703 LCK 049
LCK 114LCK 303
LCK 311LCK 339
LCK 350
LCK 353LCK 384
PO4-PPO4
CODNH4-NNH4
ClNO3-NNO3
PO4-PPO4
SO4
TOC
10 ± 130.5 ± 3500 ± 3025 ± 1.5
32.2 ± 250 ± 36 ± 0.4
26.6 ± 1.810 ± 1
30.5 ± 3500 ± 50160 ± 25
5 ± 1.515.3 ± 4.6250 ± 4012.5 ± 216.1 ± 2.625 ± 43 ± 0.5
13.3 ± 2.25 ± 1.5
15.3 ± 4.5250 ± 6080 ± 30
LCA 704 LCK 153LCK 305
LCK 311LCK 314LCK 340
LCK 349
LCK 383
SO4
NH4-NNH4
ClCODNO3-NNO3
PO4-PPO4
TOC
100 ± 155 ± 0.5
6.4 ± 0.650 ± 350 ± 625 ± 2
110.7 ± 91 ± 0.1
3.05 ± 0.316 ± 2.5
50 ± 202.5 ± 0.63.2 ± 0.7725 ± 425 ± 8
12.5 ± 2.555.4 ± 110.5 ± 0.151.53 ± 0.46
8 ± 3
LCA 700 LCK 238LCK 304
LCK 311LCK 328LCK 348
LCK 414
Ntot.
NH4-NNH4
ClKPO4-PPO4
COD
20 ± 21 ± 0.1
1,28 ± 0.1350 ± 330 ± 52,0 ± 0.26,1 ± 0.6130 ± 3
10 ± 2,50.5 ± 0.150.64 ± 0.1925 ± 415 ± 61 ± 0.25
3.05 ± 0.7615 ± 4
LCA 705 LCK 014LCK 302LCK 311
CODNH4-NNH4
Cl
5000 ± 30080 ± 10103 ± 1350 ± 3
2500 ± 40040 ± 15
51.5 ± 19.325 ± 4
LCA 706 LCK 521LCK 529LCK 537LCW032
Fetot.
Cu (II)NiMn
0,2 ± 0.030,5 ± 0.050,5 ± 0.050,5 ± 0.1
0.1 ± 0.040.25 ± 0.060.25 ± 0.060.25 ± 0.15
LCA 707 LCK 341
LCK 348totalLCK 614
NO2-NNO2
PO4-PPO4
COD
0.3 ± 0.030.99 ± 0.1
2 ± 0.26.1 ± 0.61200 ± 8
0.15 ± 0.040.5 ± 0.131 ± 0.25
3.05 ± 0.76100 ± 10
LCA 709 LCK 138LCK 342
LCK 349totalLCK 614
Ntot.
NO2-NNO2
PO4-PPO4
COD
6 ± 0.93 ± 0.3
9,85 ± 11 ± 0.1
3.05 ± 0.3200 ± 8
3 ± 1.51.5 ± 0.44.9 ± 1.30.5 ± 0.151.53 ± 0.46100 ± 10
Ntot.
PO4-PPO4
COD
60 ± 610 ± 1
30.5 ± 31000 ± 40
30 ± 85 ± 1.5
15.3 ± 4.5500 ± 50
LCA 708 LCK 338LCK 350totalLCK 514
Quality AssuranceLCA addista
Data table addista
Edition: 4/02
Test expressed as Standardnominal value max. deviation
mg/l mg/l
Spiking resultnominal value max. deviation
mg/l mg/l
GB
CODLCK 414 (5 – 60 mg/l) 3.0 LCA 700 COD 30 mg/l +/- 3 mg/l 15 mg/l +/- 4 mg/l
CODLCK 514 (100 – 2000 mg/l) – LCA 708 COD 1000 mg/l +/- 40 mg/l 500 mg/l +/- 50 mg/l
CODLCK 014 (1.000 – 10.000 mg/l) 2.5 LCA 705 COD 5000 mg/l +/- 300 mg/l 2500 mg/l +/- 400 mg/l
CODLCK 114 (150 – 1.000 mg/l) 2.0 LCA 703 COD 500 mg/l +/- 30 mg/l 250 mg/l +/- 40 mg/l
CODLCK 314 (15 – 150 mg/l) 3.0 LCA 704 COD 50 mg/l +/- 6 mg/l 25 mg/l +/- 8 mg/l
Cuvette-Test max. VC addista Evaluation Confidence Interval Confidence Interval(Measuring range) [%] as . . . nom. value of max. nom. value of max.
stand. concen. deviation spiking solut. deviation
Ammonium-NitrogenLCK 303 (2 – 47 mg/l) NH4-N 3.5 LCA 703 NH4-N 25 mg/l +/- 1.5 mg/l 12,5 mg/l +/- 2 mg/l
(2.5 – 60.0 mg/l) NH4 NH4 32.2 mg/l +/- 2 mg/l 16,1 mg/l +/- 2.6 mg/l
Ammonium-NitrogenLCK 302 (47 – 130 mg/l) NH4-N – LCA 705 NH4-N 80 mg/l +/- 10 mg/l 40 mg/l +/- 15 mg/l
(60 – 167 mg/l) NH4 NH4 103 mg/l +/- 13 mg/l 51,5 mg/l +/- 19,3 mg/l
AluminiumLCK 301 (0.02 – 0.50 mg/l) 3.0 LCA 702 Al 0.3 mg/l +/- 0.02 mg/l 0.15 mg/l +/- 0.03 mg/l
Ammonium-NitrogenLCK 304 (0.015 – 2.0 mg/l) NH4-N 3.0 LCA 700 NH4-N 1 mg/l +/- 0.1 mg/l 0.5 mg/l +/- 0.15 mg/l
(0.02 – 2.50 mg/l) NH4 NH4 1.28 mg/l +/- 0.13 mg/l 0.64 mg/l +/- 0.19 mg/l
Ammonium-NitrogenLCK 305 (1 – 12 mg/l) NH4-N 3.0 LCA 704 NH4-N 5 mg/l +/- 0.5 mg/l 2.5 mg/l +/- 0.6 mg/l
(1.3 – 15.0 mg/l) NH4 NH4 6.4 mg/l +/- 0.6 mg/l 3.2 mg/l +/- 0.77 mg/l
CadmiumLCK 308 (0.02 – 0.3 mg/l) 5.0 LCA 702 Cd 0.2 mg/l +/- 0.03 mg/l 0.1 mg/l +/- 0.04 mg/l
Chlorine/Ozone/Chlorine dioxideLCK 310 (0.05 – 2.0 mg/l) Chlorine/Ozone 3.0 – – – – – –
(0.09 – 3.8 mg/l) ClO2
ChlorideLCK 311 (1 – 70 mg/l) 3.0 LCA 700 Cl 50 mg/l +/- 3 mg/l 25 mg/l +/- 4 mg/l
LCA 703LCA 704LCA 705
Chromium (total +VI)LCK 313 (0.03 – 1.0 mg/l) 3.0 LCA 702 Cr (VI) 0.5 mg/l +/- 0.05 mg/l 0.25 mg/l +/- 0.06 mg/l
Cr tot. 0.5 mg/l +/- 0.05 mg/l 0.25 mg/l +/- 0.06 mg/l
Quality of Dr. Langeprecision Cuvette-TestsDefinitions of the used statistical data
VC: Variation coefficient [%] = precision(Procedure variation coefficient)
German standard refering to DIN 38402-A51. Scale for thedeviation in % all over the total measuring range of a specifiedtest and all over Dr. Lange’s different types of instruments.Max. VC: max. variation coefficient [%]
(max. procedure variation coefficient)
Dr. Lange companies’ internal standard concerning the abovementioned DIN but evaluated under stronger conditions.Confidence interval: scale for accuracyThe standard for addista standard should be determinedwithin this range.Max. deviation range [mg/l]:Acceptable tolerance around the addista standard-concen-tration or standard-concentration in mg/l.
PhenolsLCK 346 (5 – 50 mg/l) I 3.0 – – – – – –
(20 – 200 mg/l) II – – – – – – –
NitriteLCK 342 (0,6 – 6 mg/l) NO2-N – LCA 709 NO2-N 3 mg/l +/- 0.3 mg/l 1.5 mg/l +/- 0.4 mg/l
(2 – 20 mg/l) NO2 NO2 9.85 mg/l +/- 1 mg/l 4.9 mg/l +/- 1.3 mg/l
CODLCK 614 (50 – 300 mg/l) – LCA 707 COD 200 mg/l +/- 8 mg/l 100 mg/l +/- 10 mg/l
LCA 709
ManganeseLCW 032 (0.02 – 5.0 mg/l) – LCA 706 Mn 0.5 mg/l +/- 0.1 mg/l 0.25 mg/l +/- 0.15 mg/l
Copper 50 mm Cuvette-TestLCK 529 (0.01 – 1.0 mg/l) – LCA 706 Cu (II) 0.5 mg/l +/- 0.05 mg/l 0.25 mg/l +/- 0.06 mg/l
CopperLCK 329 (0.1 – 8.0 mg/l) 2.0 LCA 701 Cu (II) 2 mg/l +/- 0.1 mg/l 1 mg/l +/- 0.15 mg/l
FormaldehydeLCK 325 (0.5 – 10.0 mg/l) 2.0 – – – – – –
CyanideLCK 315 (0.01 – 0.6 mg/l) 5.0 – – – – – –
Cuvette-Test max. VC addista Evaluation Confidence Interval Confidence Interval(Measuring range) [%] as . . . nom. value of max. nom. value of max.
stand. concen. deviation spiking solut. deviation
LeadLCK 306 (0.1 – 2.0 mg/l) 5.0 LCA 701 Pb (II) 0.5 mg/l +/- 0.1 mg/l 0.25 mg/l +/- 0.15 mg/l
IronLCK 321 (0.2 – 6.0 mg/l) 2.0 LCA 701 Fe tot. 3 mg/l +/- 0.15 mg/l 1.5 mg/l +/- 0.2 mg/l
® Total NitrogenLCK 138 (1 – 16 mg/l) – LCA 709 Nges 6 mg/l +/- 0.9 mg/l 3 mg/l +/- 1.5 mg/lLATON
Total NitrogenLCK 238 (1 – 40 mg/l) – LCA 700 Ntot. 20 mg/l +/- 2 mg/l 10 mg/l +/- 2.5 mg/lLATON
Total NitrogenLCK 338 (20 – 100 mg/l) – LCA 708 Ntot. 60 mg/l +/- 6 mg/l 30 mg/l +/- 8 mg/lLATON
NitrateLCK 339 (0.23 – 13.5 mg/l) NO3-N 2.5 LCA 703 NO3-N 6 mg/l +/- 0.4 mg/l 3 mg/l +/- 0.5 mg/l
(1 – 60 mg/l) NO3 NO3 26.6 mg/l +/- 1.8 mg/l 13.3 mg/l +/- 2.2 mg/l
NitrateLCK 340 (5 – 35 mg/l) NO3-N 4.0 LCA 704 NO3-N 25 mg/l +/- 2 mg/l 12.5 mg/l +/- 2.5 mg/l
(22 – 155 mg/l) NO3 NO3 110.7 mg/l +/- 9 mg/l 55.4 mg/l +/- 11 mg/l
NitriteLCK 341 (0.015 – 0.6 mg/l) NO2-N 3.0 LCA 707 NO2-N 0.3 mg/l +/- 0.03 mg/l 0.15 mg/l +/- 0.04 mg/l
(0.05 – 2.0 mg/l) NO2 NO2 0.99 mg/l +/- 0.1 mg/l 0.5 mg/l +/- 0.13 mg/l
PhenolsLCK 345 (0.05 – 5.0 mg/l) 3.0 – – – – – –
Iron 50 mm Cuvette-TestLCK 521 (0.01 – 1.0 mg/l) – LCA 706 Fe tot. 0.2 mg/l +/- 0.03 mg/l 0.1 mg/l +/- 0.04 mg/l
FluorideLCK 323 (0.1 – 1.5 mg/l) 3.0 – – – – – –
MagnesiumLCK 326 (0.5 – 10.0 mg/l) I 3.5 – – – – – –
(10 – 50 mg/l) II – – – – – – –
NickelLCK 337 (0.1 – 6.0 mg/l) 2.0 LCA 701 Ni 2 mg/l +/- 0.1 mg/l 1 mg/l +/- 0.15 mg/l
Nickel 50 mm Cuvette-TestLCK 537 (0.05 – 1.0 mg/l) – LCA 706 Ni 0.5 mg/l +/- 0.05 mg/l 0.25 mg/l +/- 0.06 mg/l
Phosphate-phosphorus ortho + totalLCK 348 (0.5 – 5.0 mg/l) PO4-P 2.0 LCA 700 PO4-P 2 mg/l +/- 0.2 mg/l 1 mg/l +/- 0.25 mg/l
(1.5 – 15.0 mg/l) PO4 LCA 707 PO4 6.1 mg/l +/- 0.61 mg/l 3.05 mg/l +/- 0.76 mg/l
OrthophosphateLCK 049 (1.6 – 30 mg/l) PO4-P 2.0 LCA 703 PO4-P 10 mg/l +/- 1 mg/l 5 mg/l +/- 1.5 mg/l
(5 – 90 mg/l) PO4 PO4 30.5 mg/l +/- 3 mg/l 15.3 mg/l +/- 4.6 mg/l
SilverLCK 355 (5 – 400 mg/l) I 3.0 – – – – – –
(400 – 2500 mg/l) II – – – – – – –
Water HardnessLCK 327 (1 – 20 °dH) 5.0 – – – – – –
Phosphate-phosphorus ortho + totalLCK 349 (0.05 – 1.5 mg/l) PO4-P 1.5 LCA 704 PO4-P 1 mg/l +/- 0.1 mg/l 0.5 mg/l +/- 0.15 mg/l
(0.15 – 4.5 mg/l) PO4 LCA 709 PO4 3.05 mg/l +/- 0.3 mg/l 1.53 mg/l +/- 0.46 mg/l
Phosphate-phosphorus ortho + totalLCK 350 (2 – 20 mg/l) PO4-P 2.0 LCA 703 PO4-P 10 mg/l +/- 1 mg/l 5 mg/l +/- 1.5 mg/l
(6 – 60 mg/l) PO4 LCA 708 PO4 30.5 mg/l +/- 3 mg/l 15.3 mg/l +/- 4.5 mg/l
PotassiumLCK 328 (8 – 50 mg/l) 5.0 LCA 700 K 30 mg/l +/- 5 mg/l 15 mg/l +/- 6 mg/l
SulphateLCK 153 (40 – 150 mg/l) 5.0 LCA 704 SO4 100 mg/l +/- 15 mg/l 50 mg/l +/- 20 mg/l
SulphateLCK 353 (150 – 900 mg/l) 9.0 LCA 701 SO4 500 mg/l +/- 50 mg/l 250 mg/l +/- 60 mg/l
LCA 702LCA 703
ZincLCK 360 (0.2 – 6.0 mg/l) 3.0 LCA 701 Zn 2 mg/l +/- 0.15 mg/l 1 mg/l +/- 0.2 mg/l
Cuvette-Test max. VC addista Evaluation Confidence Interval Confidence Interval(Measuring range) [%] as . . . nom. value of max. nom. value of max.
stand. concen. deviation spiking solut. deviation
TOCLCK 383 (5 – 50 mg/l) – LCA 704 TOC 16 mg/l +/- 2.5 mg/l 8 mg/l +/- 3 mg/l
TOCLCK 384 (50 – 500 mg/l) – LCA 703 TOC 160 mg/l +/- 25 mg/l 80 mg/l +/- 30 mg/l