Expt Nichem Boren: Preliminary Data Sheet

PRELIMINARY DATA SHEET
Version:
EN LOW P BORON
Doc.-No.:
DATA SHEET SAP-No.:
EXPT NICHEM BOREN IMDS-No.:
Electroless Nickel Plating Process
CONTENTS
1. Process Information................................................................................................................................. 2
2. Typical Deposit Properties ...................................................................................................................... 2
3. Equipment ............................................................................................................................................... 3
4. Preparation of Plating Tank and Equipment ........................................................................................... 4
5. Make-Up .................................................................................................................................................. 5
6. Working Parameters ................................................................................................................................ 5
7. Plating Rate and Phosphorus Content .................................................................................................... 6
8. Maintenance ............................................................................................................................................ 6
9. pH Control ............................................................................................................................................... 7
10. Tools ........................................................................................................................................................ 8
11. General Notes ......................................................................................................................................... 8
12. Determination of Nitrate Contamination .................................................................................................. 9
13. SAP No. for Make-Up and Maintenance Products .................................................................................. 9
14. Specific Gravity for Make-Up and Maintenance Products....................................................................... 9
15. Analytical Instructions ............................................................................................................................10
Determination of Nickel by Titration.......................................................................................................10
Determination of Sodium Hypophosphite by Titration ..........................................................................12
Determination of Orthophosphite by Titration .......................................................................................14
16. Waste Disposal...........................................................................................................................166
17. General Safety Precautions ................................................................................................................166
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Version: 02
EXPT NICHEM 11 BOREN
Doc.-No.:
1. Process Information
EXPT NICHEM 11 BOREN is a metal-free stabilized electroless nickel process and therefore complies with the
international ELV regulations (End of Life Vehicle) as well as the RoHS / WEEE directive.
EXPT NICHEM 11 BOREN produces a matte surface appearance of a nickel alloy with 2 – 5 % phosphorus and
0.4-0.2% boron content.
EXPT NICHEM 11 BOREN has a high deposition rate of 15 – 20 µm/h over the whole bath life and is tolerant to
metal contamination. When proper operating parameters are followed, up to 8 MTO are attained.
EXPT NICHEM 11 BOREN is suitable for functional engineering applications that require high as-plated
hardness and good wear resistance. The deposit can be heat-treated to further increase the coating hardness.
EXPT NICHEM 11 BOREN deposit stress is moving from tensile to neutral throughout the life of the solution.
Good adhesion with the MS base material
EXPT NICHEM 11 BOREN is supplied as a four component system.
EXPT NICHEM 11 BOREN - A For make-up and replenishment. Source of Ni ions.

EXPT NICHEM 11 BOREN - B For make-up only. Source of reducer.
EXPT NICHEM 11 BOREN - C For replenishment only (ammoniated processing). Source of reducer.
EXPT NICHEM 11 BOREN - E For make-up and replenishment. Source of reducer.
2. Typical Deposit Properties
Phosphorus content (ICP) 2 – 5 % (depends on bath age and operating pH)
Hardness 750-850 HV 0.1 as deposited

1000 – 1100 HV 0.1 after heat treatment for 1 h at 400 °C
Ductility (Bend test) Passes 180°
Color matte appearance
Specific Gravity of NiP deposit 8.6 +/- 0.1
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3. Equipment
Tanks Tanks made of heat resistant plastic (e.g. PP un-pigmented or

PVDF). It is recommended to provide a two-tank-system
using one tank as reserve. (Note: Not recommended
Stainless steel 316 type tank for this chemistry).
Heating PTFE/Porcelain are recommended. It is not recommended to

exceed 2 W/cm² heat capacity.
Agitation Bath agitation is required.

Mild clean air agitation from a lower pressure blower is
recommended. If no air agitation is provided, ensure that no
overheating occurs at the heating coils. Mechanical,
reciprocal agitation is optional.
Filtration Continuous, the entire bath volume must be circulated

8-10 times per hour. Only nonmetallic pump heads should
be used.
Filter cartridges or filter bags.

Filter fineness: 1 – 5 µm (Recommended 1 µm filter pore size)
Exhaust Required due to formation of Ni aerosols and nitrous gases

while stripping with HNO3.
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4. Preparation of Plating Tank and Equipment
IMPORTANT NOTE: Never omit this stage. Before making up a new solution, it is
essential that the following steps be performed. Do not rely on visual examination.
Never take short cuts. They will always increase the cost of your electroless nickel
plating, reduce production rate and produce poor quality deposits.
1. Completely discharge spent solution to waste treatment system as per federal, state and local regulations
and permits.
2. Remove old filter cartridge(s) or bag(s) and discard. Reseal filter unit for stripping. Fully fill plating tank
over the working level with nitric acid solution (1 : 1 diluted with DI water).
Note: The Ni concentration of the stripping solution should be < 15 g/l Ni.
3. Re-circulate nitric acid solution through all pumps, filter housings, hoses, pipes, air agitation spiders and
other surfaces which normally contact the working electroless nickel solution.
Note: Do not use air agitation. The air spider should be filled with acid. If possible, allow overnight stripping
to ensure complete stripping and / or passivation of stainless steel tanks.
For increased stripping activity, the solution can be heated up to ~ 40 °C (104°F).
4. Discharge nitric acid back to holding tank for future use.
5. Pump clean water through all the hoses, filters, pumps, tanks, etc., where nitric acid was present. Rinse
thoroughly.
6. Fill tank with water to above the nitric acid level and add a small quantity of ammonium hydroxide. Circulate
this solution for 1 – 2 hours while turning the air agitator pump on and off occasionally. This will ensure that
all the nitric acid is neutralized. Nitric acid is difficult to completely remove by only rinsing.
7. Drain the system and then rinse thoroughly with clean water. Test the rinse water for nitrate (see chapter
11 of this data sheet). If no nitrate is found, continue with Step #8. If nitrate is present, continue flushing
the system with water and testing until the nitrate contamination has been eliminated.
8. Install new filter cartridges, bags etc. Ensure all new filter cartridges and bags are leached with sulfuric acid
(5 % (v/v)) if needed prior to use.
9. Repair any malfunctioning equipment or leaks that were noted during previous production cycle.
10. Recalibrate pH meters, temperature controllers, etc.
11. The equipment is now ready for make-up of a new solution.
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5. Make-Up
IMPORTANT NOTE: Always read and understand SDSs for all chemicals involved in
the make-up activity below and wear appropriate personal protective equipment.
Selection should be based upon the chemistry being used.
Make-up of 100 Liter L kg

DI water 71.5 ---
EXPT NICHEM 11 BOREN -A 5.0 approx. 6.3
EXPT NICHEM 11 BOREN -B 20.0 approx. 23.9
EXPT NICHEM 11 BOREN -E 3.5
 Fill one third of the tank volume with DI water.

 Add the required amount of EXPT NICHEM 11 BOREN - A while stirring thoroughly.
 Add the required amount of EXPT NICHEM 11 BOREN - B while stirring thoroughly.
 Add the required amount of EXPT NICHEM 11 BOREN - E while stirring thoroughly.
 Fill the tank to the final volume with DI water and mix well.
 Adjust pH to operating level 6.3 (6.25 – 6.35). (See also chapter 9)
To increase the pH, use ammonia solution 50 % (v/v); to decrease the pH, add sulfuric acid 20 % (v/v).
 Heat up to working temperature.
6. Working Parameters
Content of Nickel 5.0 g/l (4.5 – 5.5 g/l) (See also chapter 10)
An automatic nickel controller cannot be used for nickel

determination due to the blue color of the solution.
Content of Sodium hypophosphite 13 g/l (11-15 g/l)
Temperature 80 °C (79 – 81 °C)
pH 6.3 (6.25 – 6.35)

An automatic pH controller is highly recommended.
The pH has a significant influence on the phosphorus
incorporation.
Loading (area-related) 1.0 dm²/l (0.5 – 2.0 dm²/l)
Deposition rate 17 µm/h (15 – 20 µm/h)
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7. Plating Rate and Phosphorus Content
The plating rate of EXPT NICHEM 11 BOREN and the resulting phosphorus content of the deposit are primarily
a function of operating temperature, pH, reducer content and age of the solution.
Plating Phosphorus
Parameter Change
rate content
  
Temperature, pH, reducers
  
Solution age   
8. Maintenance
the maintenance activity below and wear appropriate personal protective equipment.
Regular analysis of the nickel metal content is used as the basis for additions of EXPT NICHEM 11 BOREN - A,
EXPT NICHEM 11 BOREN - C and EXPT NICHEM 11 BOREN –E. Refer to TABLE 1 for the replenishment
schedule.
EXPT NICHEM 11 BOREN -A replenishes the nickel metal in the bath. Optimum EXPT NICHEM 11 BOREN -A
concentration is 50 ml/l and this corresponds to a nickel concentration of 5.0 g/l.
To increase the nickel concentration by 1 g/l, add 10.0 ml/l of EXPT NICHEM 11 BOREN -A.
One metal turnover (MTO) is achieved when 50 ml/I of EXPT NICHEM 11 BOREN -A have been added. Per
MTO, the Orthophosphate content will increase by ~ 10 g/l.
Replenishment was done with both the reducer to maintain the concentration throughout the bath life.
Optimum EXPT NICHEM 11 BOREN -C concentration is 50 ml/l and this corresponds to a sodium
hypophosphite concentration of 13 g/l. To increase the sodium hypophosphite by 1 g/l, add 3.8 ml/l of EXPT
NICHEM 11 BOREN -C.
Optimum EXPT NICHEM 11 BOREN –E concentration is 35 ml/l and this corresponds to a dimethyl amino
borane (DMAB) concentration of 3.3 g/l.
Evaporation losses of the EN solution should be replenished with DI water (< 10 µS).
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TABLE 1
Replenishment Schedule for EXPT NICHEM 11 BOREN Bath
Nickel Content by Analysis EXPT NICHEM 11 EXPT NICHEM

EXPT NICHEM 11
BOREN -A 11 BOREN -C
BOREN –E
in ml/l in ml/l
In ml/l
100 % 5.0 g/l 0.0 0.0 0.0
95 % 4.8 g/l 2.0 2.0 1.4
90 % 4.5 g/l 5.0 5.0 3.5
85 % 4.3 g/l 7.0 7.0 5.0
80 % 4.0 g/l 10.0 10.0 7.0
75 % 3.8 g/l 12.0 12.0 8.4
70 % 3.5 g/l 15.0 15.0 10.5
It is NOT recommended to operate EXPT NICHEM 11 BOREN solutions below 90 % strength. If this occurs,
make adjustments in several small additions during the shift.
9. pH Control
The use of a properly calibrated pH meter is strongly recommended. Measurements should be made on a
sample cooled to room temperature. The mixed replenisher will hold the pH reasonably constant, but the
solution pH should be regularly checked at least once per shift and adjustments made to keep the pH within the
range 6.25 – 6.35 (6.3 optimum).
To increase the pH, use 50 % (v/v) ammonia solution. Do not use sodium or potassium hydroxide or carbonate
to adjust pH. To lower the pH, add 20 % (v/v) sulfuric acid.
Operating the EXPT NICHEM 11 BOREN bath outside the recommended pH range has the following adverse
effects:
 Poor deposit quality - color, roughness, ductility, adhesion, etc.

 Solution instability - too high pH may cause spontaneous breakdown of the solution.
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10. Tools
In some applications, the use of tools can be necessary. Please consult an Atotech representative before using
tools.
 Nichem WA:
For the reduction of surface tension which prevents formation of pores and pitting.
For details refer to the TDS of EXPT NICHEM WA (SAP No.: 1679370).
11. General Notes
Maintenance additions should be made as frequently as possible so that the optimum plating rate and deposit
characteristics are obtained.
It is NOT recommended to operate EXPT NICHEM 11 BOREN solutions below 90 % strength. If this occurs,
make adjustments in several small additions during the shift.
As in all plating procedures, proper cleaning/activation of basis metals is essential. Contact your local Atotech
representative for specific procedures and cycles.
EXPT NICHEM 11 BOREN is tolerant to many impurities; however, all electroless nickel solutions are adversely
affected by drag-in of specific impurities, e.g. Al, Fe, Zn, Cr, Cu, Cd, Pb, Sn, organo-sulfur compounds and
certain surface-active materials.
To minimize the drag-in of impurities into the EN tank, it is recommended to use DI water in the last rinse before
the EN tank.
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12. Determination of Nitrate Contamination
Nitrate contamination of electroless nickel baths will cause slow plating rates and produce deposits having lower
than normal phosphorus contents. Such contamination most often occurs after the tank has been etched with
nitric acid and the tank, piping and associated equipment is improperly rinsed with water.
Ion selective papers are available which allow nitrate to be determined in both the EN plating solution and in the
®¹
make-up water in the range of 10 – 500 mg/l. These strips are manufactured by EM QUANT and are available
from VWR Scientific Products.
¹ A registered trademark of Merck KGaA.
13. SAP No. for Make-Up and Maintenance Products
PRODUCT SAP No.

EXPT NICHEM 11 BOREN -A 1689708
EXPT NICHEM 11 BOREN –B 1689709
EXPT NICHEM 11 BOREN –C 1689710
EXPT NICHEM 11 BOREN –E 1689773
NICHEM® WA 1685105
14. Specific Gravity for Make-Up and Maintenance Products
PRODUCT SG (g/cm³)
EXPT NICHEM 11 BOREN -A 1.250
EXPT NICHEM 11 BOREN -B 1.144
EXPT NICHEM 11 BOREN -C 1.154
EXPT NICHEM 11 BOREN –E 0.96
NICHEM WA 1.005
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15. Analytical Instructions
the analytical activity below and wear appropriate personal protective equipment.
Version:
Determination of Nickel by Titration Doc.-No.:
*
Reagent required
 Ammonia conc.
 Murexide indicator solution (1 : 200 ground with NaCl)
 0.1 M EDTA volumetric solution
Please follow the general regulations for hazardous materials in the SDSs!
The analytical procedure is to be followed exactly.
Be sure to observe all local regulations concerning the permitted limits for
pollutants.
Procedure

**
5.0 ml nickel bath are pipetted into a 300 ml Erlenmeyer flask. Add
 100 ml DI water, 10 ml ammonia conc. and 1 spatula tip murexide indicator solution.

***
Titrate with 0.1 M EDTA volumetric solution until the color of the solution changes
from yellow to violet-blue.
The number of ml of 0.1 M EDTA volumetric solution used – multiplied by 1.174 – gives the content of nickel in
g/l.
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Example:
During titration of 5.0 ml bath, 5.1 ml of 0.1 M EDTA solution was used.
Calculation:
5.1 x 1.174 = 6.0 g/l Nickel
Quality assurance: For maintenance, calibration of measuring devices and the use of
standards and reference materials, please refer to the corresponding guidelines.
* Unless otherwise stated, these are always analytical grade substances.

** Volumes given exact to a decimal point must be measured with a volumetric pipette.
*** For the purposes of calculation, the factor of the volumetric solutions is assumed to be 1.000
and is therefore not taken into account in the examples.
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Version:
Determination of Sodium Hypophosphite by Titration Doc.-No.:
Principle: Redox titration
Reagents required*:
 Hydrochloric acid 6 M; (6 N); 500 ml/l HCl 37 %, density 1.19 g/cm³

 Iodine volumetric solution 0.05 M (0.1 N)
 Sodium thiosulfate volumetric solution 0.1 M (0.1 N); 24.818 g/l Na2S2O3  5 H2O
 Indicator: Starch solution 1 % (shortly boiled!)
pollutants.
Procedure:
 To 25 ml of 6 M Hydrochloric acid in a 250 ml iodine flask

 1.0 ml** of the sample and
 20.0** ml of 0.05 M iodine volumetric solution are added. Afterwards, the flask is placed sealed in the dark
for 30 min. Then the solution is filled up with approx. 100 ml DI water and is titrated with
 0.1 M sodium thiosulfate volumetric solution, until the color changes from brown to bright yellow. After an
addition of 1 ml of the starch solution, the solution is titrated again, until the dark blue color completely
disappears.
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Calculation:
ml 0.1 M Na2S2O3-volumetric solution)  5.3 = sodium

*** ***
(original 0.05 M I2-volumetric solution – consumed
hypophosphite  H2O in g/l
Example:
During titration of 1.0 ml sample, 14.2 ml of 0.1 M Na2S2O3-volumetric solution was used.
(20.0 – 14.2)  5.3 = 30.7 g/l sodium hypophosphite  H2O

*** For the purpose of calculation, the factor of the standard solution is assumed to be 1.000 and is therefore
not taken into account in the examples.
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Version:
Determination of Orthophosphite by Titration Doc.-No.:
Reagents required*:
 Iodine volumetric solution 0.05 M (0.1 N)

 Sodium thiosulfate volumetric solution 0.1 M (0.1 N); 24.818 g/l Na 2S2O3  H2O
 Sodium hydrogen carbonate solution 5 %
 Acetic acid 10 %
 Indicator: Starch solution 1 % (shortly boiled!)
pollutants.
Procedure:

1)
1.0 ml**of the sample is placed into a 250 ml iodine flask and add
 approx. 80 ml of DI water,
 20 ml of sodium hydrogen carbonate solution and
 25.0 ml** of 0.05 M iodine volumetric solution. Afterwards, place it closed in the dark for 30 min. Then add
 20 ml of acetic acid and titrate with
 0.1 M sodium thiosulfate volumetric solution, until the color changes from brown to bright-yellow. After an
addition of
 1 ml of the starch solution, the solution is titrated with 0.1 M sodium thiosulfate volumetric solution, until the
dark blue color in the solution completely disappeared.
1)
With the chosen volumes. a determination of orthophosphite is possible to approx. 90 g/l.
With higher contents, the sample volume must be cut in half and the calculation factor must
be doubled correspondingly.
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Calculation:
0.1 M sodium thiosulfate-volumetric solution)  4

*** ***
(original 0.05 M iodine volumetric solution – consumed
2-
gives the content of HPO3 (orthophosphite) in g/l.
Example:
During titration of 1.0 ml sample, 5.8 ml of 0.1 M sodium thiosulfate volumetric solution was used.
(25.0 – 5.8)  4 = 76.8 g/l HPO3 (orthophosphite)

2-
During titration of 0.5 ml sample, 12.0 ml of 0.1 M sodium thiosulfate volumetric solution was used.
(25.0 – 12.0)  8 = 104.0 g/l HPO3 (orthophosphite)

2-

*** For the purpose of calculation, the factor of the standard solution is assumed to be 1.000 and is therefore not
taken into account in the examples.
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16. Waste Disposal
This material must be disposed of in accordance with all applicable federal, state, provincial, and local
regulations and permits. Consult the SDS for additional regulatory information. The information contained herein
is general in nature and may not apply to each application.
17. General Safety Precautions

When working with this product(s), ensure that all health, environmental, and safety regulations and standards
are met. Avoid direct contact with this material. Do not inhale associated mist, vapors, and/or dust. Maintain and
limit exposure as recommended by OSHA, ACGIH, and other state/provincial and local regulations. Wash
contaminated clothing before reuse. Always comply with the Hazard Communication Standard, 29 CFR
1910.1200 and Workplace Hazardous Materials Information System. Emergency showers and eyewashes must
be readily available. Wear the appropriate personal protective equipment for the chemistry being handled.
It is recommended that the plating chemistry product(s) referred to in this Technical Information Sheet be used:
(a) in accordance with the information provided in product specific SDS; and (b) in compliance with all applicable
requirements and guidelines established by OSHA, NIOSH, ACGIH, NFPA, and others.
NOTE: A Safety Data Sheet (SDS) for this product(s) is available upon request from Atotech USA, LLC,
Customer Service/Sales Support Group, 1750 Overview Drive, Rock Hill, SC 29730.
REVIEW SDS BEFORE USING THIS PLATING CHEMISTRY AND FOR SPECIFIC INFORMATION.
A precautionary approach should be used when there is potential for chemical exposure -- this includes
minimizing exposure potential, rapid decontamination, and medical follow-up.
This sheet shall serve for your information. The content of the sheet is based on our best Atotech Deutschland GmbH
knowledge. We do not undertake any duty to advise. The contents of the sheet shall not P.O. Box: 21 07 80
be considered as an agreement on condition and quality of the goods delivered. 10507 Berlin, Germany
The decision to use our products for its production purposes is the responsibility of our Erasmusstraße 20
customer. We can accept liability only for the quality of our products at delivery. If 10553 Berlin, Germany
difficulties arise in the application of our products, we propose that you contact our phone +49 (0) 30 349 85 0
technical service department. fax +49 (0) 30 349 85 777
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PRELIMINARY DATA SHEET

EXPT NICHEM BOREN IMDS-No.:

Electroless Nickel Plating Process

Released on: Released by:

EXPT NICHEM 11 BOREN is supplied as a four component system.

EXPT NICHEM 11 BOREN - A For make-up and replenishment. Source of Ni ions.

2. Typical Deposit Properties

Phosphorus content (ICP) 2 – 5 % (depends on bath age and operating pH)

Hardness 750-850 HV 0.1 as deposited

Ductility (Bend test) Passes 180°

Color matte appearance

Specific Gravity of NiP deposit 8.6 +/- 0.1

Released on: Released by:

14.02.2017 GMF USA

Tanks Tanks made of heat resistant plastic (e.g. PP un-pigmented or

Heating PTFE/Porcelain are recommended. It is not recommended to

Agitation Bath agitation is required.

Filtration Continuous, the entire bath volume must be circulated

Filter cartridges or filter bags.

Exhaust Required due to formation of Ni aerosols and nitrous gases

Released on: Released by:

14.02.2017 GMF USA

4. Preparation of Plating Tank and Equipment

4. Discharge nitric acid back to holding tank for future use.

10. Recalibrate pH meters, temperature controllers, etc.

11. The equipment is now ready for make-up of a new solution.

Released on: Released by:

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Make-up of 100 Liter L kg

 Fill one third of the tank volume with DI water.

An automatic nickel controller cannot be used for nickel

Content of Sodium hypophosphite 13 g/l (11-15 g/l)

Temperature 80 °C (79 – 81 °C)

pH 6.3 (6.25 – 6.35)

Loading (area-related) 1.0 dm²/l (0.5 – 2.0 dm²/l)

Deposition rate 17 µm/h (15 – 20 µm/h)

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7. Plating Rate and Phosphorus Content

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Nickel Content by Analysis EXPT NICHEM 11 EXPT NICHEM

 Poor deposit quality - color, roughness, ductility, adhesion, etc.

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11. General Notes

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12. Determination of Nitrate Contamination

¹ A registered trademark of Merck KGaA.

13. SAP No. for Make-Up and Maintenance Products

PRODUCT SAP No.

14. Specific Gravity for Make-Up and Maintenance Products

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15. Analytical Instructions

Determination of Nickel by Titration Doc.-No.:

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5.1 x 1.174 = 6.0 g/l Nickel

* Unless otherwise stated, these are always analytical grade substances.

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