View
212
Download
0
Category
Preview:
Citation preview
8/20/2019 HACH Cloruros
http://slidepdf.com/reader/full/hach-cloruros 1/6
Chloride
Page 1 of 6
Chloride, 8113
How to use instrument-specific information
The Instrument-specific information table displays requirements that may vary between
instruments. To use this table, select an instrument then read across to find the corresponding
information required to perform this test.
Chloride DOC316.53.01017
Mercuric Thiocyanate Method Method 8113
(0.1 to 25.0 mg/L Cl –)
Scope and Application: For water and wastewater
Test preparation
Table 81 Instrument-specific information
Instrument Sample cell Cell orientation
DR 6000 2495402 Fill line faces right
DR 5000 2495402 Fill line faces user
DR 3900 2495402 Fill line faces user
DR 3800, DR 2800, DR 2700 2495402 Fill line faces right
Before starting the test:
Filter turbid samples with moderately rapid filter paper and a funnel before analysis.
Both the sample and the blank will contain mercury (D009) at a concentration regulated as a hazardous waste by the Federal
RCRA. Do not pour these solutions down the drain.
Refer to the MSDS sheet for safe handling and disposal of hazardous waste. Gloves are recommended.
Collect the following items:
Description Quantity
Ferric Ion Solution 1 mL
Mercuric Thiocyanate Solution 2 mL
Deionized Water 10 mL
Sample Cells (see Instrument-specific information) 2
Pipet, TenSette®, 0.1 to 1.0 mL 1
Pipet tips for 0.1 to 1.0 mL TenSette pipet 2
See Consumables and replacement items for reorder information.
8/20/2019 HACH Cloruros
http://slidepdf.com/reader/full/hach-cloruros 2/6
Chloride
Page 2 of 6
Chloride
Mercuric Thiocyanate method for Chloride
1. Select the test.
Insert an adapter if
required (Instrument-
specific information).
Refer to the user manual
for orientation.
2. Prepared Sample:
Fill a sample cell with
10 mL of sample.
3. Blank Preparation:
Fill another sample cell
with 10 mL of deionized
water.
4. Pipet 0.8 mL of
Mercuric Thiocyanate
Solution into each sample
cell. Note: Use 1.0 mL
with DR 5000 .
5. Swirl to mix. 6. Pipet 0.4 mL of Ferric
Ion Solution into eachsample cell. Not e: Use 0.5
mL with DR 5000 .
7. Swirl to mix. An
orange color will develop ifchloride is present.
8. Start the instrument
timer. A two-minute reaction time
will begin.
9. Within five minutes
after the timer expires,
wipe the blank and insert it
into the cell holder.
10. ZERO the instrument.
The display will show:
0.0 mg/L Cl –
11. Wipe the prepared
sample and insert it into
the cell holder.
12. READ the results in
mg/L Cl –.
70 Chloride
Stored Programs
Start
Zero Read
8/20/2019 HACH Cloruros
http://slidepdf.com/reader/full/hach-cloruros 3/6
Chloride
Chloride
Page 3 of 6
Interferences
Sample collection, preservation and storage
Collect samples in glass or plastic containers. Samples can be stored for at least 28 days at room
temperature.
Accuracy check
Required for accuracy check:
• Chloride Standard Solution, 1000-mg/L
• 50 mL mixing cylinders (3)
• TenSette Pipet and tips
Standard additions method (sample spike)
1. After reading test results, leave the sample cell (unspiked sample) in the instrument.
2. Select Options>More>Standard additions from the instrument menu.
3. Default values for standard concentration, sample volume, and spike volumes can be
accepted or edited. After values are accepted, the unspiked sample reading will appear in the
top row. See the user manual for more information.
4. Prepare three sample spikes. Fill three 50 mL mixing cylinders with 50 mL of sample. Use the
TenSette® Pipet to add 0.1 mL, 0.2 mL and 0.3 mL of 1000-mg/L Chloride Standard Solution,
respectively, to the cylinders and mix each thoroughly.
5. Analyze a 10 mL portion of each sample spike as described in the Mercuric Thiocyanate
method for Chloride test, starting with the 0.1 mL sample spike. Each addition should reflect
approximately 100% recovery.
6. Select GRAPH to view the results. Select IDEAL LINE (or best-fit) to compare the standard
addition results to the theoretical 100% recovery.
Standard Solution Method
Required for accuracy check:• Chloride Standard Solution, 1000-mg/L
• Volumetric Flask, 500-mL
• Pipet, Class A, 10 mL
1. Prepare a 20.0-mg/L chloride standard solution.
a. Pipet 10.00 mL of Chloride Standard Solution, 1000-mg/L, into a 500-mL volumetric flask.
b. Dilute to the mark with deionized water. Follow the Mercuric Thiocyanate method for
Chloride test.
Table 82 Interfering substances and levels
Interfering substance Interference levels and treatments
Extreme pH
The pH should be about 2 after adding reagents.
If the sample is strongly acidic or alkaline, adjust a portion of sample before testing to a pH of
about 7. Use either 5.0 N Sodium Hydroxide Standard Solution1 or a 1:5 dilution of perchloric acid.Use pH paper ; most pH electrodes will contaminate the sample with chloride.
1 See Optional reagents and apparatus.
8/20/2019 HACH Cloruros
http://slidepdf.com/reader/full/hach-cloruros 4/6
Chloride
Page 4 of 6
Chloride
2. To adjust the calibration curve using the reading obtained with the standard solution, select
Options>More>Standard Adjust from the instrument menu.
3. Turn on the Standard Adjust feature and accept the displayed concentration. If an alternate
concentration is used, enter the concentration and adjust the curve to that value.
Method performance
Summary of method
Chloride in the sample reacts with mercuric thiocyanate to form mercuric chloride and liberate
thiocyanate ion. Thiocyanate ions react with the ferric ions to form an orange ferric thiocyanatecomplex. The amount of this complex is proportional to the chloride concentration. Test results are
measured at 455 nm.
Consumables and replacement items
Program Standard
Precision
95% Confidence Limits of
Distribution
Sensitivity
Concentration change
per 0.010 Abs change
Portion of curve
70 20.0 mg/L Cl – 17.9–22.1 mg/L Cl – 0.1 mg/L Cl – 1.0 mg/L
0.3 mg/L Cl – 10.0 mg/L
0.6 mg/L Cl – 20.0 mg/L
Required reagents
Description Quantity/Test Unit Catalog number
Chloride Reagent Set, includes: — 250 tests/pkg1
1 This test requires a reagent blank. The number of tests shown refers to any combination of samples and blanks.
2319800
(1) Ferric Ion Solution 1 mL 100 mL 2212242
(1) Mercuric Thiocyanate Solution 2 mL 200 mL 2212129
Water, deionized 10 mL 4 L 27256
Required apparatus
Description Quantity Unit Catalog number
Pipet, TenSette®, 0.1 to 1.0 mL 1 each 1970001
Pipet Tips, for TenSette Pipet 1970001 varies 50/pkg 2185696
Sample cell, 10 mL square, matched pair 2 2/pkg 2495402
Recommended standards
Description Unit Catalog number
Chloride Standard Solution, 1000-mg/L Cl – 500 mL 18349
8/20/2019 HACH Cloruros
http://slidepdf.com/reader/full/hach-cloruros 5/6
Chloride
Chloride
Page 5 of 6
Optional reagents and apparatus
Description Unit Catalog number
Chloride Standard Solution, 10-mL Voluette® Ampule, 12,500-mg/L Cl – 16/pkg 1425010
Chloride Standard Solution, 100-mg/L Cl – 1 L 2370853
Cylinder, mixing, 50 mL each 189641
Filter Paper, funnel, 125 mm 100/pkg 69257
Funnel, poly, 75 mm each 108368
Gloves, chemical resistant, size 9–9.51
1 Other sizes available
pair 2410104
Perchloric Acid, ACS 680 g 75765
pH Paper, 1.0–11.0 pH range, 15 foot roll 5/pkg 39133
Pipet Tips, for TenSette Pipet 1970001 1000/pkg 2185628
Pipet, volumetric, Class A, 10 mL each 1451538
Pipet Filler, safety bulb each 1465100
Sodium Hydroxide Standard Solution, 5.0 N 50 mL 245026
Voluette Ampule Breaker, for 10-mL ampules each 2196800
8/20/2019 HACH Cloruros
http://slidepdf.com/reader/full/hach-cloruros 6/6
HACH COMPANYWORLD HEADQUARTERSTelephone: (970) 669-3050
FAX: (970) 669-2932
FOR TECHNICAL ASSISTANCE, PRICE INFORMATION AND ORDERING:Call 800-227-4224
Contact the HACH office or distributor serving you.
www.hach.com techhelp@hach.com
In the U.S.A. –
Outside the U.S.A. –
On the Worldwide Web – ; E-mail –
toll-free
© Hach Company, 2007, 2010, 2012. All rights reserved. Printed in the U.S.A. Edition 7
Recommended